Device and method for analytically and sensorily determining the release of active ingredients from a delivery system
By designing equipment and methods for capsules or precursors, releasing active ingredients using physical or chemical stimulation, and combining detection devices, the subjectivity and irregularity problems of analysis in the prior art are solved, and quantitative and qualitative analysis are achieved. Improves the speed and repeatability of the analysis.
Patent Information
- Application Number
- CN201980103505.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2019-11-27
- Publication Date
- 2024-12-24
- Estimated Expiration
- 2039-11-27
AI Technical Summary
In the prior art, methods for determining the release of active ingredients from capsules or precursors are subjective and irregular, making objective, qualitative and quantitative analysis difficult, and there is a lack of fast and repeatable methods.
A device and method is designed to release active ingredients from capsules or precursors through physical or chemical stimuli (such as pressure, friction, UV radiation) and use detection devices to perform qualitative and quantitative analysis to achieve standardized analytical methods.
Quantitative and qualitative analysis of active ingredients is achieved, reproducible and rapid release characteristic curve determination, capable of measuring release rates and characteristics online, and improves the evaluation of mechanical stability and fracture strength of capsules and precursors.
Smart Images

Figure CN115003343B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a device and a method for determining the release of one or more active ingredients from a release system in an analytical and / or sensory manner. In particular, the invention relates to a device and a method for determining the release of one or more active ingredients, in particular aroma substances or taste substances or aroma substance mixtures or aroma mixtures, from capsules or precursors. In addition, the invention relates to a device and a method for determining the properties of a release system, in particular a capsule or a precursor. Finally, the invention relates to the use of the device according to the invention and the method according to the invention for determining the release of one or more active ingredients from a release system in an analytical and / or sensory manner.
[0002] In the sense of the present invention, a delivery system is a solid preparation, for example microparticles or capsules, which comprises one active ingredient or several active ingredients.
[0003] Another example of such a release system is a so-called precursor or precursor substance. In the case of such a precursor or precursor substance, one or more active ingredients are released by chemical or physical stimulation, for example by chemical reaction with reagents, temperature, humidity, pH value change, oxygen (oxidation), light such as UV radiation, enzymes, microorganisms, etc. For example, when making fragrances, the precursor is a molecule with a weaker own odor, and when external factors such as temperature, oxygen (oxidation), light, enzymes, microorganisms, chemical reactions (such as hydrolysis), pH value changes or humidity act on the molecule, the molecule releases at least one new fragrance molecule. Thus, in the life cycle of such a fragrance precursor, new fragrance notes are always released and easily changing odors are formed.
[0004] The person skilled in the art generally understands the term "encapsulation" as a technology by which finely divided solid, liquid or gaseous substances, for example active ingredients, are surrounded and thereby immobilized by a film-forming shell formed from polymeric and / or inorganic wall materials.
[0005] The substance or active ingredient enclosed within the capsule is often referred to as the core material.
[0006] Thus, individual properties of the microcapsules can be achieved, depending on the wall or shell material and the degree of crosslinking.
[0007] The aim here is to protect the active ingredient, referred to as the active principle, before any reaction with the environment, such as moisture or oxidation, and also before any reaction with other substances and / or to be able to release the active ingredient in a targeted manner at a defined point in time.
[0008] During encapsulation, they are classified into matrix capsules or core / shell capsules according to the phase morphology. In matrix encapsulation, the active ingredient is uniformly blended with the shell component ("matrix") and microparticles are produced, in which the active ingredient is uniformly distributed. Matrix systems are also referred to as microparticles. The release of the active ingredient / active ingredients is usually carried out by diffusion of the active ingredient into the environment or by degradation of the matrix.
[0009] In core / shell packaging, the active ingredient constituting the core is wrapped with a shell material. A real capsule with one or more shells is produced. Generally speaking, mechanical stresses such as pressure or shearing forces produce a complete release of the core material. However, it is also possible to release the core material or the active ingredient in a targeted manner by alternative opening mechanisms such as temperature, pH changes, UV radiation, microwaves or ultrasound.
[0010] In addition to macroscopic particles with diameters in the range of up to 1 cm, microcapsules are of particular interest. The person skilled in the art understands these as spherical particles with a diameter in the range of about 0.0001 to about 5 mm and preferably 0.005 to 0.5 mm.
[0011] According to the present invention, the term "microcapsule" is understood to be microparticles and aggregates containing an inner space or core, which is filled with a solid, gelled, liquid or gaseous medium and is surrounded (encapsulated) by a continuous shell formed by a film-forming polymer. In addition, microscopically smaller capsules may contain one or more cores distributed in a continuous encapsulating material composed of one or more sublayers.
[0012] The shell of such microcapsules can be made up of natural, semi-synthetic or synthetic materials. Natural shell materials are, for example, gum arabic, agar, agarose, maltodextrin, alginic acid or its salts, for example, sodium alginate or calcium alginate, fat and fatty acid, cetyl alcohol, collagen, chitosan, lecithin, gelatin, albumin, shellac, polysaccharides such as starch or dextran, polypeptide, protein hydrolyzate, sucrose and wax. Semi-synthetic shell materials are, in particular, chemically modified cellulose, in particular cellulose esters and ethers such as ethyl cellulose, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and carboxymethyl cellulose, and starch derivatives, in particular starch ethers and esters. Synthetic shell materials are, for example, polymers such as polyacrylates, polyamides, polyvinyl alcohol, aminoplasts, phenolic plastics or polyvinyl pyrrolidone.
[0013] This results in flexible application possibilities depending on the use of the various wall and core materials.
[0014] The preparation of microcapsules has been described in detail in the literature of the prior art and can be obtained with the aid of known reactive and non-reactive methods, such as solvent evaporation, precipitation, coacervation, interfacial polycondensation, high pressure encapsulation processes and the like.
[0015] Examples of prior art microcapsules are the following commercial products (shell materials are given in parentheses): Hallcrest Microcapsules (gelatin, gum arabic), Coletica Thalaspheres (marine collagen), Lipotec Millicapseln (alginic acid, agar), Induchem Unispheres (lactose, microcrystalline cellulose, hydroxypropyl methylcellulose); Unicerin C30 (lactose, microcrystalline cellulose, hydroxypropyl methylcellulose), Kobo Glycospheres (modified starch, fatty acid esters, phospholipids), Softspheres (modified agar) and Kuhs Probiol Nanospheres (phospholipids) as well as Primaspheres and Primasponges (chitosan, alginate) and Primasys (phospholipids). As well as capsules formed from synthetic polymers (BASF), Microcapsules 500 and 560 (Koehler SE), Folco
[0016] Due to their properties, capsules, in particular microcapsules, comprising one or more active ingredients are used in particular in the printing industry (e.g. scented lacquers), the food industry (e.g. vitamins, aromas, plant extracts, enzymes, microorganisms), agrochemistry (e.g. fertilizers, plant protection agents), the feed industry (e.g. minerals, vitamins, enzymes, medicaments, microorganisms), the pharmaceutical industry, the cleaning agent industry and the cosmetics industry.
[0017] Nowadays, many items of daily needs, such as detergents, softeners, washing powders, washing liquids, shower gels, shampoos, deodorants, body lotions, etc., are scented with encapsulated fragrance substances or fragrance substance mixtures.
[0018] In particular, the capsules, preferably the microcapsules, are used for the preparation of, for example, perfume absolutes, perfumes, eau de toilettes, aftershaves, colognes, preshave products, cologne sprays, acidic, alkaline and neutral cleaners, for example floor cleaners, window cleaners, dishwashing detergents, bathroom and toilet cleaners, cleaning milks, solid and liquid toilet cleaners, powdered and foamed carpet cleaners, liquid detergents, powdered detergents, laundry pretreatment agents such as bleaches, softeners and stain removers, fabric softeners, cleaning soaps, cleaning tablets, disinfectants, surface disinfectants and air fresheners in liquid, gel or applied to a solid carrier, aerosol sprays, waxes and polishes, such as furniture polishes, floor waxes, shoe polishes and body care agents, such as solid and liquid soaps, shower gels, shampoos, shaving soaps , shaving foam, bath oil, cosmetic emulsions of the oil-in-water, water-in-oil and water-in-oil-in-water type such as skin creams and lotions, face cleansers and lotions, sunscreen creams and lotions, after-sun creams and lotions, hand creams and lotions, foot creams and lotions, depilatory creams and lotions, aftershave creams and lotions, tanning creams and lotions, hair care products such as hair sprays, gels, setting lotions, conditioners, permanent and semi-permanent hair dyes, hair texturizing agents such as cold wave lotions and straighteners, hair root nourishing lotions, hair creams and lotions, deodorants and antiperspirants such as armpit sprays, roll-ons, deodorant sticks, deodorant creams or decorative cosmetic products such as eye shadow, nail polish, make-up, lipstick, mascara, wet wipes, cleaning wipes, baby cleaning wipes, intimate cleaning wipes, candles, lamp oil, incense sticks, insecticides, insect repellents, fuel.
[0019] The use of a suitable shell material to encapsulate an active ingredient or ingredients may be used for a variety of reasons:
[0020] -Converting liquids into a processable powder form (e.g. encapsulating vegetable oils, fats);
[0021] - time-controlled or delayed release of substances (dose control, storage effect in the case of medicaments, plant protection agents and fertilizers);
[0022] - stacking of tastes, smells and colours (e.g. more bitter or spicier aromas);
[0023] -Protection against light, oxidation, heat, acid or alkali (e.g. vitamins, aromatic substances, etc.)
[0024] - Protection against moisture, e.g. hygroscopic salts or minerals;
[0025] - Reduce the evaporation rate of volatile components (such as aromatic substances);
[0026] - prevent premature chemical reactions with other mixture components;
[0027] - better handleability before or during processing (e.g. optimized flow characteristics, avoidance of fine dust formation);
[0028] - protect persons from materials that are harmful to health or unpleasant to the sense of smell (chemicals, aromatic concentrates); or
[0029] - Better dispersibility.
[0030] Special uses of microcapsules are, for example, detergents and cleaning agents for the controlled or delayed release of fragrance substances onto textile surfaces. During washing, the microcapsules containing fragrance substances or perfume oils are distributed on the laundry and adhere to the fabric. When the clothes are worn, due to the friction or pressure that occurs, the capsules burst and release the fragrance substance or perfume oil.
[0031] The contents of the microcapsules can be released in various ways. Four typical mechanisms can be considered here:
[0032] Mechanical destruction of the capsule wall by crushing or shearing. This mechanism is used, for example, in reactive carbonless writing papers.
[0033] - Destruction of the capsule wall by melting of the wall material. According to this mechanism, for example in baking mixes, the contents (such as leavening agents or flavoring agents) are released only during the baking process.
[0034] - Destruction of the capsule wall by dissolution of the wall material. This mechanism works, for example, in the case of washing powders, whereby the encapsulated contents (such as enzymes) are only released during the washing process.
[0035] - The capsule remains unchanged and the capsule contents are gradually released through the capsule wall by diffusion. According to this mechanism, for example, a slow and uniform release of the active ingredient of a pharmaceutical agent can be achieved in the body.
[0036] In order to be able to take appropriate measures when developing, preparing and using such active ingredient release systems, especially capsules or precursors, it is important to obtain information about the release of the active ingredients, such as the concentration of one or more active ingredients, the release rate, the release profile of one or more active ingredients, etc., as well as information about their properties, such as the mechanical stability of the capsule shell, the breaking strength, the hysteresis behavior, etc.
[0037] Currently, the release of one or more active ingredients, in particular aroma or taste substances, from capsules, in particular microcapsules, is determined by sensory-analytical scoring using various methods, using specifically trained testers / panels.
[0038] Descriptive perceptual analysis, i.e. methods that describe perceptual properties, are among the most demanding perceptual methods due to their flexibility and complexity. These methods are traditionally based on the perceptual perception of appropriately qualified personnel, produce detailed product profiles, but are time- and cost-intensive. For tasks within the scope of classic descriptive analysis, such as the identification, description and quantification of subjectively perceptible product properties, testers with special skills are used. The goal of this method is to obtain a detailed product description that can be compared with other products or can also be converted into a product recipe. In addition to the multi-stage perceptual methods, complex training methods for tester certification are a key focus in classic perceptual analysis.
[0039] Cost and time pressures in innovation as well as ever-shorter product life cycles increasingly require faster presentation of decision-relevant information. Short-time methods, so-called rapid description methods, can form an alternative in this respect, since these methods also allow the use of untrained testers, but are associated with information losses.
[0040] Although the trend is to standardize perception ratings, either through improved methodology or through better training of testers, ratings are still subjective and should not be equated with objective or standardized analytical methods based on specific metrics.
[0041] In sensory analysis, the active ingredient is usually released from a release system, especially a capsule, by manual abrasion without standardizing the pressure, such as the pressure, applied to the release system, especially the capsule, so that the results of the release of the active ingredient are subject to large fluctuations.
[0042] The main object of the present invention is therefore to overcome the above-mentioned problems and to provide a device and a method for carrying out an objective and normalized (that is to say standardized) analysis method, which can reproducibly, qualitatively and / or quantitatively draw conclusions about the release of one or more active ingredients, in particular qualitatively and / or quantitatively draw conclusions about the released active ingredients and / or about the properties of the active ingredient release system, in particular the capsule.
[0043] In particular, it is an object of the present invention to provide a standardized method for analytically and / or sensorily determining the release of one or more active ingredients from a release system, in particular from a capsule or a precursor.
[0044] Furthermore, it is an object of the present invention to design the device in a simple manner and to be able to use the method in a simple manner and to be able to use it variably for a large number of different release systems or active ingredients.
[0045] Finally, it is an object of the invention to make the device combinable with standard analytical instruments in order to enable identification and quantitative measurement.
[0046] Surprisingly, it has been found that the above-mentioned purpose can be achieved by a device and / or a method, in which one or more active ingredients are released from a release system 6, preferably from a capsule 6 or a precursor 6, by physical or chemical stimulation, such as pressure and / or friction, and the released active ingredient or the released active ingredients are fed to a detection device and finally the released active ingredients are determined analytically.
[0047] The process technology advantage is that the device and / or method according to the invention provides an objective analysis method under normalized (i.e. standardized) conditions, which allows, for example, the analysis values of various release systems to be compared with each other and the release of the active ingredient can be measured continuously online.
[0048] The device according to the invention and the method according to the invention make it possible in particular to determine the concentration of the active ingredient released, to determine the release rate of the active ingredient or to determine the release profile of one or more active ingredients.
[0049] On the other hand, the device according to the invention and the method according to the invention allow the determination of properties of a release system, in particular a capsule, such as the mechanical stability and breaking strength of the capsule or, for example, the hysteresis behavior of the capsule after a certain period of storage.
[0050] The device and the method of the present invention can also be used to: test the distribution and adhesion of a release system, especially a capsule (6) or a precursor (6), on a substrate, and / or analyze the affinity of one or more active ingredients on a substrate after release from the release system (6), especially the capsule (6) or the precursor (6); and / or to analyze the influence of physical or chemical factors such as temperature, light, UV radiation, pH value on the mechanical stability and breaking strength of the release system and / or on the release of one or more active ingredients from the release system; and / or to test the release of one or more active ingredients and the characteristics of the release system during the development and preparation of the release system. Summary of the invention
[0051] In a first aspect, the invention relates to a device 1 suitable for analytically and / or sensory determination of the release of one or more active ingredients from a release system 6, in particular a capsule 6 or a precursor 6 and / or for determining the properties of a release system 6, in particular a capsule 6 or a precursor 6, the release system / capsule / precursor being located on a sample carrier 7 or a support surface 8, the device comprising:
[0052] (a) Basic frame 2;
[0053] (b) an activation device 3 connected to the base frame 2 and adapted to open or activate the release system 6, in particular the capsule 6 or the precursor 6, and release the active ingredient or the active ingredients contained therein;
[0054] as well as
[0055] (c) A detection device 5 adapted for analytically determining the released active ingredient and designed to be able to deliver the released active ingredient or the released active ingredients to the detection device 5 .
[0056] In another aspect, the present invention relates to a method for analytically and / or sensory determination of the release of an active ingredient or multiple active ingredients from a release system 6, in particular a capsule 6 or a precursor 6 and / or for determining the properties of a release system 6, in particular a capsule 6 or a precursor 6, comprising the following steps:
[0057] (i) providing a release system 6, in particular a capsule 6 or a precursor 6, on a sample carrier 7 or a support surface 8, wherein the release system / capsule / precursor comprises one active ingredient or multiple active ingredients;
[0058] (ii) positioning an activation device 3 with an activator 31 above the release system 6, in particular the capsule 6 or the precursor 6;
[0059] (iii) lowering the activation device 3;
[0060] (iv) releasing the active ingredient or the plurality of active ingredients from the release system 6, in particular the capsule 6 or the precursor 6, by means of the activator 31;
[0061] (v) collecting the released active ingredients and sending them to the detection device 5; and
[0062] (vi) Analytically determining the released active ingredient.
[0063] Finally, the invention is directed to the use of the device according to the invention and of the method according to the invention,
[0064] - for determining the release of one or more active ingredients from a release system 6, in particular a capsule 6 or a precursor 6, in an analytical and / or sensory manner, in particular determining the concentration, the release rate or the release profile;
[0065] - for determining the properties of the release system 6, in particular the capsule 6 or the precursor 6, such as determining the mechanical stability, the breaking strength or the hysteresis behavior, in particular determining the mechanical stability, the breaking strength or the hysteresis behavior of capsules 6 formed from different capsule materials and different active ingredients;
[0066] - for analyzing the distribution and adhesion of the release system 6, in particular the capsules 6 or the precursors 6, on the substrate, in particular after washing and drying the textile;
[0067] - for analyzing the affinity of an active ingredient or multiple active ingredients on a substrate after release from the release system 6, in particular the capsule 6 or the precursor 6;
[0068] - for analyzing the influence of physical or chemical factors such as temperature, light, UV radiation, pH value on the mechanical stability and breaking strength of the release system, in particular the capsule or precursor 6 and / or on the release of one or more active ingredients from the release system 6, in particular the capsule 6 or the precursor 6;
[0069] For analytically determining the release of an active ingredient or several active ingredients and for determining properties of a release system 6 , in particular a capsule 6 or a precursor 6 , during the production of the release system 6 .
[0070] For those skilled in the art, these and other aspects, features and advantages of the present invention can be derived from the study of the following detailed description and claims. Here, any feature from one aspect of the present invention can theoretically be used in any other aspect of the present invention. In addition, it is self-evident that the embodiments contained herein describe and illustrate the present invention, but these embodiments should not limit the present invention, and the present invention is especially not limited to these embodiments.
[0071] As used in the context of this specification, the term "at least one" refers to one or more, such as one, two, three, four, five, six, seven, eight, nine or more. Thus, the term "at least one positioning unit" for example means obtaining at least one positioning unit, but may also include two or more positioning units. BRIEF DESCRIPTION OF THE DRAWINGS
[0072] Figure 1 A schematic top view of a preferred variant of the device according to the invention is shown.
[0073] Figure 2 A schematic cross section through a preferred variant of an activation device of the device according to the invention is shown.
[0074] Figure 3 A perspective detail view of a preferred variant of the device according to the invention is shown.
[0075] Figure 4 A preferred variant of the device according to the invention is shown in a perspective view in an overview with a detection system and a delivery catheter.
[0076] Figure 5 Schematic diagram showing the steps of the analytical method according to the present invention.
[0077] Figure 6 An exemplary curve of continuous measurement of capsule bursting of capsules containing perfume oil is shown.
[0078] Figure 7 Shown is a comparison of the fragrance release of methylformamide based core / shell perfume oil capsules having different wall thicknesses. DETAILED DESCRIPTION
[0079] In the following, reference is made to the Figures 1 to 4 The device of the present invention, its variants and preferred embodiments thereof are described in detail.
[0080] The device 1 provided for analytical and / or sensory determination is not only used for analytically determining the release of one or more active ingredients from a capsule, but is also typically configured for analytically and / or sensory determination of the release of one or more active ingredients from a release system comprising or containing the active ingredient.
[0081] In the context of the present invention, a release system is understood to be a solid preparation, such as microparticles or capsules, comprising one or more active ingredients. A preferred release system is a capsule, preferably a microcapsule of a matrix type or a core / shell type. In the matrix encapsulation, the active ingredient is uniformly blended with a shell component ("matrix") and microparticles are produced, in which the active ingredient is uniformly distributed. The release of the active ingredient from this capsule type is usually carried out by diffusion of the active ingredient into the environment or by the degradation rate of the matrix. In the core / shell encapsulation, the active ingredient constituting the core is wrapped with a shell material. A real capsule with one or more shells is produced. Generally speaking, mechanical stresses such as pressure or shear force produce the complete release of the core material. But it is also possible to release the core material in a targeted manner by alternative opening mechanisms such as temperature, pH value, UV light, microwaves or ultrasound.
[0082] In connection with the present invention, a device 1 according to the invention which is suitable for analytically determining the release of active ingredients from capsules, for example from hard capsules, soft capsules (soft shell capsules), macrocapsules, microcapsules, capsule slurries and capsule emulsions is particularly preferred.
[0083] In the context of the present invention, a release system is also understood to be a precursor or precursor substance. Such precursors or precursor substances release one or more active ingredients by chemical or physical stimulation, for example by temperature, oxygen (oxidation), light, enzymes, microorganisms, chemical reactions (such as hydrolysis), pH changes or moisture, etc. The precursors used according to the invention are, for example, fragrance substances with a weaker own odor, which release at least one new fragrance molecule when they are associated with external factors such as light, water or oxygen. Thus, new fragrance notes are always released during the life cycle of the fragrance and an easily variable smell is formed.
[0084] In the context of the present invention, the term "release system" preferably includes capsules, especially microcapsules, and also precursors or precursor substances. The terms "release system", "capsule", "microcapsule", "precursor or precursor substance" are used in the following description equivalently and interchangeably, so that one term can simultaneously include the other term and vice versa. The terms "capsule" and "microcapsule" include not only capsules of the matrix type but also capsules of the core / shell type.
[0085] In a first aspect, the invention therefore relates to a device 1 for analytically and / or sensorily determining the release of an active ingredient or ingredients from a release system 6, preferably from a capsule 6 or a precursor.
[0086] Release is understood to mean the release or generation of the active ingredient from the formulation, ie from the release system 6 , preferably the capsule 6 or the precursor 6 .
[0087] Analytically measuring is generally understood to mean qualitatively (identification of the active ingredient) and / or quantitatively (amount of the active ingredient) analyzing the active ingredient released or generated from the release system 6, in particular the active ingredient or the active ingredients released or generated from the capsule 6 or the precursor 6. By means of analytically measuring, the concentration of the released active ingredient and the release rate, that is to say the release of the active ingredient over time, can be determined.
[0088] When determining the release rate, it is measured how, ie with what intensity and / or in what concentration, the active ingredient or the active ingredients are released from the capsule over time.
[0089] Furthermore, the release profile can also be determined qualitatively and quantitatively by analytical determination, that is to say the rapid or delayed release of one or more active ingredients. The determination of the release profile is particularly important in the case of mixtures of active ingredients, for example perfume oils, fragrance mixtures or flavor mixtures. With the aid of the release profile, it can be determined how (that is to say with what intensity and / or in what concentration) the individual components of the fragrance mixture or flavor mixture are released over time from the release system, in particular from the capsule 6 or from the precursor 6.
[0090] Furthermore, the device 1 is configured for determining properties of a release system 6, in particular a capsule 6. Determining properties of a release system is understood to mean analyzing functional properties, such as mechanical stability, breaking strength or hysteresis behavior, in particular after storage of the release system or capsule for a certain period of time.
[0091] By analyzing the released active ingredients, information can be obtained about the concentration of the released active ingredients, about the release rate of the active ingredients (rapid release vs. delayed release), about the release characteristic curve of, for example, a mixture of active ingredients, or about the stability of the capsule shell, about what kind of bursting behavior (rupture behavior) the capsule shell has, about the hysteresis properties of the capsule shell (for example after the release system has been stored for a certain period of time), etc.
[0092] In the release system 6, preferably in the capsule 6, the material distributed in the matrix or the contained core material or active ingredient is a solid, liquid or gaseous substance. The core material of the release system 6 is preferably a volatile substance that can volatilize at room temperature.
[0093] The selection of the active ingredient used in the above-mentioned delivery system is basically in accordance with the application purpose that the delivery system is to meet.
[0094] In the release system 6, preferably the capsule 6, active ingredients from the following areas are preferably used: detergents and cleaners, glues, coating compositions such as colorants and paints, adhesives, such as materials for plastics, paper, textiles, lubricants, building materials, dyes, organic and inorganic powders, pigment dispersions, phase change materials, fire retardants, agricultural chemicals, and also active ingredients from the cosmetic and pharmaceutical fields.
[0095] The release system 6, preferably the capsule 6, preferably contains at least one active ingredient selected from the group consisting of aroma substances, flavor substances, perfume oils, aroma substance mixtures, fragrances, vitamins, minerals, antioxidants, anthocyanins, coenzyme IO, glues, mineral oils, waxes and fats, biocides, fungicides, herbicides, pesticides, insecticides, fertilizers, dispersion dyes and dye solutions or monomers for the synthesis of plastics.
[0096] The active ingredient or active ingredients are preferably fragrance substances, flavor substances, perfume oils, fragrance substance mixtures or aromatic substances. These active ingredients are generally volatile substances that can volatilize at room temperature.
[0097] Preferably, the aroma or flavor substances or aroma or flavor mixtures comprising two, three, four, five or even more aroma or flavor components are selected from the group consisting of: (1) hydrocarbons; (2) aliphatic alcohols; (3) aliphatic aldehydes and their acetals; (4) aliphatic ketones and their oximes; (5) aliphatic sulfur compounds; (6) aliphatic nitriles; (7) esters of aliphatic carboxylic acids; (8) acyclic terpene alcohols; (9) acyclic terpene aldehydes and terpene ketones; (10) cyclic terpene alcohols; (11) cyclic terpene aldehydes and terpene ketones; (12) cyclic alcohols; (13) cycloaliphatic alcohols; (14) cyclic and cycloaliphatic (15) cyclic and macrocyclic ketones; (16) cycloaliphatic aldehydes; (17) cycloaliphatic ketones; (18) esters of cyclic alcohols; (19) esters of cycloaliphatic alcohols; (20) esters of cycloaliphatic carboxylic acids; (21) aromatic aliphatic alcohols; (22) esters of aromatic aliphatic alcohols with aliphatic carboxylic acids; (23) aromatic aliphatic ethers; (24) aromatic and aromatic aliphatic aldehydes; (25) aromatic and aromatic aliphatic ketones; (26) aromatic and aromatic aliphatic carboxylic acids and their esters; (27) nitrogen-containing aromatic compounds; (28) phenols, phenyl ethers and phenyl esters; (29) heterocyclic compounds; (30) lactones; and any mixtures thereof.
[0098] The selection of aroma or flavor substances is very extensive here; corresponding substances can be found, for example, in “S. Arctander, Perfume and Flavor Chemicals, Band I and II, Montclair, NJ, 1969, Eigenverlag” or “H. Surburg and J. Panten, Common Fragrance and Flavor Materials, 6. Ausgabe, Wiley-VCH, Weinheim, 2016”.
[0099] Specifically, the following can be mentioned:
[0100] Extracts of natural raw materials: This group represents essential oils, extracts, absolutes, resins, resinoids, gums, tinctures, for example, ambergris tincture; balsam oil; angelica seed oil; angelica root oil; anise oil; valerian oil; basil oil; tree moss absolute; bay leaf oil; wormwood oil; benzoin resin; bergamot oil; beeswax absolute; birch tar; bitter almond oil; savory oil; buchu leaf oil; balsam oil; juniper oil; calamus oil; camphor oil; ylang ylang oil; cardamom oil; balsam bark oil; black currant oil; black currant absolute; castoreum absolute; cypress leaf oil; cypress wood oil; labdanum oil; citronella oil; lemon oil; copaiba balsam; copaiba balsam oil; coriander oil; ginger root oil; cumin oil; cypress oil; indigo oil; dill weed oil; dill seed oil; bitter Neroli leaf water absolute; Oakmoss absolute; Elemi resin oil; Tarragon oil; Lemon eucalyptus oil; Eucalyptus oil; Fennel oil; Spruce needle oil; Galbanum oil; Galbanum resin; Geranium oil; Grapefruit oil; Guaiac wood oil; Guyun balm; Guyun balm oil; Helichrysum absolute; Helichrysum oil; Ginger oil; Iris root absolute; Iris root oil; Jasmine absolute; Calamus oil; Chamomile oil, blue; Chamomile oil, Roman; Carrot seed oil; Balsam bark oil; Pine needle oil; Spearmint oil; Caraway oil; Lavender oil; Lavender absolute; Lavender oil; Lavender absolute; Lavender oil; Lemongrass oil; Lovage oil; Distilled lime oil; Pressed lime oil; Camphor oil; Litsea cubeba oil; Bay leaf oil; Nutmeg oil Marjoram oil; Mandarin oil; Masson pine oil; Mimosa absolute; Musk granules; Musk tincture; Clary sage oil; Nutmeg oil Myrrh Absolute; Myrrh Oil; Myrtle Oil; Carnation Leaf Oil; Carnation Flower Oil; Neroli Oil; Frankincense Absolute; Frankincense Oil; Acacia Oil; Neroli Absolute; Orange Oil; Oregano Oil; Palmarosa Oil; Patchouli Oil; Perilla Oil; Peruvian Balm Oil; Parsley Leaf Oil; Parsley Seed Oil; Petitgrain Oil; Peppermint Oil; Peppermint Oil; Pine Oil; Porridge Oil Rose absolute; rosewood oil; rose oil; rosemary oil; sage oil, Dalmatian; sage oil, Spanish; sandalwood oil; celery seed oil; lavender oil; anise oil; benzoin oil; marigold oil; fir needle oil; tea tree oil; rosin oil; thyme oil; tolu balsam; tonka absolute; tuberose absolute; vanilla extract; violet leaf absolute; verbena oil; vetiver oil; juniper berry oil; wine yeast oil; wormwood oil; wintergreen oil; ylang-ylang oil; hyssop flower oil; civet absolute; cinnamon leaf oil; cinnamon bark oil and fractions thereof, or fractions isolated therefrom.
[0101] Individual aroma substances: Individual aroma substances can be subdivided into several categories, namely:
[0102] Hydrocarbons, for example 3-carene; α-pinene; β-pinene; α-terpene; γ-terpene; p-cymene; bisabolol; camphene; caryophyllene; cedrene; afarnesene; limonene; longifolene; myrcene; ocimene; valencia citriene; (E,Z)-1,3,5-undecatriene; styrene; diphenylmethane;
[0103] Fatty alcohols such as hexanol; octanol; 3-octanol; 2,6-dimethylheptanol; 2-methyl-2-heptanol; 2-methyl-2-octanol; (E)-2-hexenol; (E)- and (Z)-3-hexenol; 1-octen-3-ol; a mixture of 3,4,5,6,6-pentamethyl-3 / 4-hepten-2-ol and 3,5,6,6-tetramethyl-4-methyleneheptan-2-ol (E,Z)-2,6-nonadienol; 3,7-dimethyl-7-methoxyoctan-2-ol; 9-decenol; 10-undecenol; 4-methyl-3-decen-5-ol;
[0104] Aliphatic aldehydes and acetals thereof, for example hexanal; heptanal; octanal; nonanal; decanal; undecanal; dodecanal; tridecanal; 2-methyloctanal; 2-methylnonanal; (E)-2-hexenal; (Z)-4-heptenal; 2,6-dimethyl-5-heptenal; 10-undecenal; (E)-4-decenal; 2-dodecenal; 2,6,10-trimethyl-9-undecenal; 2,6,10-trimethyl-5,9-undecadienal; heptaldehyde diethyl acetal; 1,1-dimethoxy-2,2,5-trimethyl-4-hexene; citronellyloxyacetaldehyde; 1-(1-methoxy-propoxy)-(E,Z)-3-hexene;
[0105] Aliphatic ketones and their ketoximes, for example 2-heptanone; 2-octanone; 3-octanone; 2-nonanone; 5-methyl-3-heptanone; 5-methyl-3-heptanone oxime; 2,4,4,7-tetramethyl-6-octen-3-one; 6-methyl-5-hepten-2-one;
[0106] Aliphatic sulfur compounds, such as 3-methylthiohexanol; 3-methylthiohexyl acetate; 3-mercaptohexanol; 3-mercaptohexyl acetate; 3-mercaptohexyl butyrate; 3-acetylthiohexyl acetate; 1-menthene-8-thiol;
[0107] Aliphatic nitriles, for example 2-nonenoic acid nitrile; 2-undecenoic acid nitrile; 2-tridecenoic acid nitrile; 3,12-tridecadienoic acid nitrile; 3,7-dimethyl-2,6-octadienoic acid nitrile; 3,7-dimethyl-6-octenoic acid nitrile;
[0108] Esters of aliphatic carboxylic acids, for example (E)- and (Z)-3-hexenyl carboxylate; ethyl acetoacetate; isoamyl acetate; hexyl acetate; 3,5,5-trimethylhexyl acetate; 3-methyl-2-butenyl acetate; (E)-2-hexenyl acetate; (E)- and (Z)-3-hexenyl acetate; octyl acetate; 3-octyl acetate; 1-octen-3-yl acetate; ethyl butyrate; butyl butyrate; isoamyl butyrate; hexyl butyrate Esters; (E)- and (Z)-3-hexenyl isobutyrate; hexyl crotonate; ethyl isovalerate; ethyl 2-methylpentanoate; ethyl hexanoate; allyl hexanoate; ethyl heptanoate; allyl heptanoate; ethyl octanoate; ethyl (E,Z)-2,4-decadienoate; methyl 2-octynoate; methyl 2-nonynoate; allyl 2-isopentyloxyacetate; methyl-3,7-dimethyl-2,6-octadienoate; 4-methyl-2-pentyl-crotonate;
[0109] acyclic terpene alcohols, for example citronellol; geraniol; nerol; linalool; lavandulol; nerolidol; farnesol; tetrahydrolinalool; tetrahydrogeraniol; 2,6-dimethyl-7-octen-2-ol; 2,6-dimethyloctan-2-ol; 2-methyl-6-methylene-7-octen-2-ol; 2,6-dimethyl-5,7-octadien-2-ol; 2,6-dimethyl-3,5-octadien-2-ol; 3,7-dimethyl-4,6-octadien-3-ol; 3,7-dimethyl-1,5,7-octatrien-3-ol; 2,6-dimethyl-2,5,7-octatrien-1-ol; and their formates, acetates, propionates, isobutyrates, butyrates, isovalerates, valerates, hexanoates, crotonates, tiglic acid esters and 3-methyl-2-butenoate esters;
[0110] Acyclic terpene aldehydes and terpene ketones, such as geranial; neral; citronellal; 7-hydroxy-3,7-dimethyloctanal; 7-methoxy-3,7-dimethyloctanal; 2,6,10-trimethyl-9-undecenal; geranylacetone; and the dimethyl acetal and diethyl acetal of geranial, neral and 7-hydroxy-3,7-dimethyloctanal;
[0111] Cyclic terpene alcohols, for example menthol; isopulegol; α-terpineol; terpineol-4; menthan-8-ol; menthan-1-ol; menthan-7-ol; bornyl alcohol; isobornyl alcohol; linalool oxide; knopol; cedrol; ambroxanol; vetiverol; guaiacol; and their formates, acetates, propionates, isobutyrates, butyrates, isovalerates, valerates, hexanoates, crotonates, tiglic acid esters and 3-methyl-2-butenoates;
[0112] Cyclic terpene aldehydes and terpene ketones, for example menthone; isomenthone; 8-mercaptomenthan-3-one; carvone; camphor; fenchone; α-ionone; β-ionone; α-n-methylionone; β-n-methylionone; α-isomethylionone; β-isomethylionone; α-ferroxene; α-damascenone; β-damascenone; β-damascenone; δ-damascenone; γ-damascenone; 1-(2,4,4-trimethyl-2-cyclohexene- 1-yl)-2-buten-1-one; 1,3,4,6,7,8a-hexahydro-1,1,5,5-tetramethyl-2H-2,4a-methyl-bridged naphthalene-8(5H)-one; 2-methyl-4-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2-butenal; nootkatone; dihydronootkatone; 4,6,8-megatrien-3-one; α-sweet orange aldehyde; β-sweet orange aldehyde; acylated cedarwood oil (methyl cedarwood ketone);
[0113] Cyclic alcohols, for example 4-tert-butylcyclohexanol; 3,3,5-trimethylcyclohexanol; 3-isocamphorylcyclohexanol; 2,6,9-trimethyl-Z2,Z5,E9-cyclododecatrien-1-ol; 2-isobutyl-4-methyltetrahydro-2H-pyran-4-ol;
[0114] Cycloaliphatic alcohols, for example α,3,3-trimethylcyclohexylmethanol; 1-(4-isopropylcyclohexyl)ethanol; 2-methyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)butanol; 2-methyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol; 2-ethyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol; 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol; -(2,2,3-trimethyl-3-cyclopenten-1-yl)-pentan-2-ol; 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-4-penten-2-ol; 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-4-penten-2-ol; 1-(2,2,6-trimethylcyclohexyl)pentan-3-ol; 1-(2,2,6-trimethylcyclohexyl)hexan-3-ol;
[0115] Cyclic and cycloaliphatic ethers, for example eucalyptol; cedryl methyl ether; cyclododecyl methyl ether; 1,1-dimethoxycyclododecane; (ethoxymethoxy)cyclododecane; α-cedryl oxide 3a,6,6,9a-tetramethyldodecahydronaphtho[2,1-b]furan; 3a-ethyl-6,6,9a-trimethyldodecahydronaphtho[2,1-b]furan; 1,5,9-trimethyl-13-oxabicyclo[10.1.0]trideca-4,8-diene; rose oxide; 2-(2,4-dimethyl-3-cyclohexen-1-yl)-5-methyl-5-(1-methylpropyl)-1,3-dioxane;
[0116] Cyclic and macrocyclic ketones, for example 4-tert-butylcyclohexanone; 2,2,5-trimethyl-5-pentylcyclopentanone; 2-heptylcyclopentanone; 2-pentylcyclopentanone; 2-hydroxy-3-methyl-2-cyclopenten-1-one; 3-methyl-cis-2-penten-1-yl-2-cyclopenten-1-one; 3-methyl-2-pentyl-2-cyclopenten-1-one; 3-methyl-4-cyclopentadecenone; 3-Methyl-5-cyclopentadecenone; 3-methylcyclopentadecanone; 4-(1-ethoxyvinyl)-3,3,5,5-tetramethylcyclohexanone; 4-tert-pentylcyclohexanone; 5-cyclohexadecene-1-one; 6,7-dihydro-1,1,2,3,3-pentamethyl-4(5H)-indanone; 8-cyclohexadecene-1-one; 9-cycloheptadecene-1-one; cyclopentadecanone; cyclohexadecanone;
[0117] Cycloaliphatic aldehydes, for example 2,4-dimethyl-3-cyclohexenecarboxaldehyde; 2-methyl-4-(2,2,6-trimethyl-cyclohexen-1-yl)-2-butenal; 4-(4-hydroxy-4-methylpentyl)-3-cyclohexenecarboxaldehyde; 4-(4-methyl-3-penten-1-yl)-3-cyclohexenecarboxaldehyde;
[0118] Cycloaliphatic ketones, for example 1-(3,3-dimethylcyclohexyl)-4-penten-1-one; 2,2-dimethyl-1-(2,4-dimethyl-3-cyclohexen-1-yl)-1-propanone; 1-(5,5-dimethyl-1-cyclohexen-1-yl)-4-penten-1-one; 2,3,8,8-tetramethyl-1,2,3,4,5,6,7,8-octahydro-2-naphthene-1 methyl ketone; methyl-2,6,10-trimethyl-2,5,9-cyclododecatrienyl ketone; tert-butyl-(2,4-dimethyl-3-cyclohexen-1-yl) ketone;
[0119] Esters of cyclic alcohols, for example 2-tert-butyl cyclohexyl acetate; 4-tert-butyl cyclohexyl acetate; 2-tert-pentyl cyclohexyl acetate; 4-tert-pentyl cyclohexyl acetate; 3,3,5-trimethylcyclohexyl acetate; decahydro-2-naphthyl acetate; 2-cyclopentylcyclopentyl crotonate; 3-pentyltetrahydro-2H-pyran-4-yl acetate; decahydro-2,5,5,8a-tetrahydro- Methyl-2-naphthyl acetate; 4,7-methano-3a,4,5,6,7,7a-hexahydro-5 or 6-indenyl acetate; 4,7-methano-3a,4,5,6,7,7a-hexahydro-5 or 6-indenyl propionate; 4,7-methano-3a,4,5,6,7,7a-hexahydro-5 or 6-indenyl isobutyrate; 4,7-methanooctahydro-5 or 6-indenyl acetate;
[0120] Esters of cycloaliphatic alcohols, for example 1-cyclohexylethyl crotonate;
[0121] Esters of cycloaliphatic carboxylic acids, for example allyl-3-cyclohexylpropionate; allyl cyclohexyloxyacetate; cis- and trans-methyldihydrojasmonate; cis- and trans-methyljasmonate; methyl-2-hexyl-3-oxocyclopentanecarboxylate; ethyl-2-ethyl-6,6-dimethyl-2-cyclohexenecarboxylate; ethyl-2,3,6,6-tetramethyl-2-cyclohexenecarboxylate; ethyl-2-methyl-1,3-dioxolane-2-acetate;
[0122] Aromatic aliphatic alcohols such as benzyl alcohol; 1-phenylethyl alcohol; 2-phenylethyl alcohol; 3-phenylpropanol; 2-phenylpropanol; 2-phenoxyethanol; 2,2-dimethyl-3-phenylpropanol; 2,2-dimethyl-3-(3-methylphenyl)propanol; 1,1-dimethyl-2-phenylethyl alcohol; 1,1-dimethyl-3-phenylpropanol; 1-ethyl-1-methyl-3-phenylpropanol; 2-methyl-5-phenylpentanol; 3-methyl-5-phenylpentanol; 3-phenyl-2-propen-1-ol; 4-methoxybenzyl alcohol; 1-(4-isopropylphenyl)ethanol;
[0123] Esters of aromatic aliphatic alcohols with aliphatic carboxylic acids, for example, benzyl acetate; benzyl propionate; benzyl isobutyrate; benzyl isovalerate; 2-phenylethyl acetate; 2-phenylethyl propionate; 2-phenylethyl isobutyrate; 2-phenylethyl isovalerate; 1-phenylethyl acetate; α-trichloromethylbenzyl acetate; α,α-dimethylphenylethyl acetate; α,α-dimethylphenylethyl butyrate; cinnamyl acetate; 2-phenoxyethyl isobutyrate; 4-methoxybenzyl acetate;
[0124] Aromatic aliphatic ethers, for example 2-phenylethyl methyl ether; 2-phenylethyl isopentyl ether; 2-phenylethyl-1-ethoxyethyl ether; phenylacetaldehyde dimethyl acetal; phenylacetaldehyde diethyl acetal; hydrogenated atroaldehyde dimethyl acetal; phenylacetaldehyde glycerol acetal; 2,4,6-trimethyl-4-phenyl-1,3-dioxane; 4,4a,5,9b-tetrahydroindeno[1,2-d]-m-dioxin; 4,4a,5,9b-tetrahydro-2,4-dimethylindeno[1,2-d]-m-dioxin;
[0125] Aromatic and aromatic aliphatic aldehydes, for example benzaldehyde; phenylacetaldehyde; 3-phenylpropanal; hydroataldehyde; 4-methylbenzaldehyde; 4-methylphenylacetaldehyde; 3-(4-ethylphenyl)-2,2-dimethylpropanal; 2-methyl-3-(4-isopropylphenyl)propanal; 2-methyl-3-(4-tert-butylphenyl)propanal; 2-methyl-3-(4-isobutylphenyl)propanal; 3-(4-tert-butylphenyl)propanal ; Cinnamaldehyde; α-butylcinnamaldehyde; α-amylcinnamaldehyde; α-hexylcinnamaldehyde; 3-methyl-5-phenylpentanal; 4-methoxybenzaldehyde; 4-hydroxy-3-methoxybenzaldehyde; 4-hydroxy-3-ethoxybenzaldehyde; 3,4-methylenedioxybenzaldehyde; 3,4-dimethoxybenzaldehyde; 2-methyl-3-(4-methoxyphenyl)propanal; 2-methyl-3-(4-methylenedioxyphenyl)propanal;
[0126] Aromatic and aromatic aliphatic ketones, for example acetophenone; 4-methylacetophenone; 4-methoxyacetophenone; 4-tert-butyl-2,6-dimethylacetophenone; 4-phenyl-2-butanone; 4-(4-hydroxyphenyl)-2-butanone; 1-(2-naphthyl)ethanone; 2-benzofuranylethanone; (3-methyl-2-benzofuranyl)ethanone; benzophenone; 1,1,2,3,3,6-hexamethyl-5-indanylmethyl ketone; 6-tert-butyl-1,1-dimethyl-4-indanylmethyl ketone; 1-[2,3-dihydro-1,1,2,6-tetramethyl-3-(1-methylethyl)-1H-5-indenyl]ethanone; 5',6',7',8'-tetrahydro-3',5',5',6',8',8'-hexamethyl-2-naphthylacetonone;
[0127] Aromatic and aromatic aliphatic carboxylic acids and their esters, for example benzoic acid; phenylacetic acid; methyl benzoate; ethyl benzoate; hexyl benzoate; benzyl benzoate; methyl phenyl acetate; ethyl phenyl acetate; geranyl phenyl acetate; phenylethyl-phenyl acetate; methyl cinnamate; ethyl cinnamate; benzyl cinnamate; phenylethyl cinnamate; cinnamyl cinnamate; allylphenoxyacetate; methyl salicylate; isopentyl salicylate; hexyl salicylate; cyclohexyl salicylate; cis-3-hexenyl salicylate; benzyl salicylate; phenylethyl salicylate; methyl-2,4-dihydroxy-3,6-dimethylbenzoate; ethyl-3-phenylglycerate; ethyl-3-methyl-3-phenylglycerate;
[0128] Aromatic nitrogen compounds, for example 2,4,6-trinitro-1,3-dimethyl-5-tert-butylbenzene; 3,5-dinitro-2,6-dimethyl-4-tert-butylacetophenone; cinnamic acid nitrile; 3-methyl-5-phenyl-2-pentenoic acid nitrile; 3-methyl-5-phenylvaleric acid nitrile; methyl aminobenzoate; methyl-N-methylaminobenzoate; Schiff bases of methyl aminobenzoate with 7-hydroxy-3,7-dimethyloctanal, 2-methyl-3-(4-tert-butylphenyl)propanal or 2,4-dimethyl-3-cyclohexenecarboxaldehyde; 6-isopropylquinoline; 6-isobutylquinoline; 6-sec-butylquinoline; 2-(3-phenylpropyl)pyridine; indole; skatole; 2-methoxy-3-isopropylpyrazine; 2-isobutyl-3-methoxypyrazine;
[0129] Phenols, phenyl ethers and phenyl esters, for example estragole; anethole; eugenol; eugenol methyl ether; isoeugenol; isoeugenol methyl ether; thymol; carvacrol; diphenyl ether; β-naphthyl methyl ether; β-naphthyl ethyl ether; β-naphthyl isobutyl ether; 1,4-dimethoxybenzene; eugenol acetate; 2-methoxy-4-methylphenol; 2-ethoxy-5-(1-propenyl)phenol; p-tolylphenyl acetate;
[0130] Heterocyclic compounds, for example 2,5-dimethyl-4-hydroxy-2H-furan-3-one; 2-ethyl-4-hydroxy-5-methyl-2H-furan-3-one; 3-hydroxy-2-methyl-4H-pyran-4-one; 2-ethyl-3-hydroxy-4H-pyran-4-one;
[0131] Lactones, such as 1,4-octanolactone; 3-methyl-1,4-octanolactone; 1,4-nonanolactone; 1,4-decanolactone; 8-decene-1,4-lactone; 1,4-undecanolactone; 1,4-dodecanolactone; 1,5-decanolactone; 1,5-dodecanolactone; 4-methyl-1,4-decanolactone; 1,15-pentadecanolactone; cis- and trans-11-pentadecanolactone; cis- and trans-11-pentadecanolactone Formula: 12-pentadecadecene-1,15-lactone; 1,16-hexadecene-lactone; 9-hexadecene-1,16-lactone; 10-oxa-1,16-hexadecene-lactone; 11-oxa-1,16-hexadecene-lactone; 12-oxa-1,16-hexadecene-lactone; 1,12-dodecanoic acid vinyl ester; 1,13-tridecanedioic acid vinyl ester; coumarin; 2,3-dihydrocoumarin; octahydrocoumarin;
[0132] And any mixture of the above aroma substances or taste substances.
[0133] Equally suitable and preferably as active ingredient is so-called precursor compound or precursor, preferably fragrance substance precursor or fragrance substance precursor.Such compound is by breaking chemical bond, for example by chemical reaction, temperature, humidity, pH value change, oxygen (oxidation), light especially UV light, enzyme or microorganism release desired odor molecule and / or fragrance substance molecule compound.Typically, in order to form fragrance substance precursor, desired fragrance substance raw material is chemically connected with carrier, preferably slightly volatile or medium volatile carrier.This combination produces the fragrance substance precursor with lower volatility and stronger hydrophobicity of improved material affinity.Then release fragrance substance, for example by pH value change (for example by transpiration when wearing), humidity, heat and / or sunlight during storage or during drying on clothesline by breaking the bond between fragrance substance raw material and carrier to release fragrance substance.
[0134] Such fragrance precursors or fragrance precursors are described, for example, in Herrmann, Andreas, Controlled release of volatiles under mild reaction conditions: from nature to everyday products, Angew. Chem., Int. Ed., 2007, 46, pages 2-30, the disclosure of which is hereby fully incorporated into the present application by reference.
[0135] The device 1 according to the invention preferably consists of a base frame 2. The base frame may be of any form and configuration adapted for receiving the activation device (3).
[0136] In a preferred variant of the device according to the invention, the base frame comprises at least one X-axis 21 and one Y-axis 22. In a more preferred variant, the base frame 2 consists of two legs extending parallel to each other. The X-axis 21 is preferably supported on the base frame at an angle of 90° and is adapted to move the activation device 3 horizontally and in the X direction relative to the support surface 8 or the plane in which the sample to be analyzed is located. The device according to the invention preferably has two X-axes 21 spaced apart from each other and supported in parallel on the base frame.
[0137] A Y-axis 22 is thus preferably mounted at an angle of 90° on the two X-axes 21 and is adapted to move the activation device 3 horizontally and in the Y direction relative to the support surface 8 or the plane in which the sample to be analyzed lies.
[0138] By means of the two X-axes 21 and the Y-axis 22 , the activation device 3 can be set to predetermined coordinates on the sample carrier 7 or the support surface 8 directly on which the sample lies, or can be moved in the direction towards the sample 6 to be analyzed and positioned exactly above the sample.
[0139] According to a first aspect of the invention, the device 1 for determining an active ingredient or multiple active ingredients from a release system 6, especially a capsule 6 or a precursor 6 in an analytical and / or sensory manner also includes an activation device 3. The activation device 3 is used to open, for example, break or activate the release system 6, especially the capsule 6 or the precursor 6, so as to release the active ingredient or the multiple active ingredients from the release system. The activation device of the device of the present invention is preferably arranged at the base frame 2, especially at the Y-axis 22 and connected thereto. In order to move and position relative to the sample 6, the activation device 3 is fastened to the base frame 2, especially in a three-dimensionally free manner.
[0140] The activation device 3 is moved and positioned horizontally and in X and Y position relative to the sample carrier 7 or relative to the support surface 8 on which the sample 6 to be analyzed (i.e. the release system 6) is located by means of an X / Y positioning unit (41; 42). The positioning unit is a drive that can be used to set the coordinates of the activation device 3 manually or via an EDV-controlled motor. The positioning unit is preferably a motor that controls the coordinates of the sample 6 to be analyzed by means of an EDV controller and positions the activation device 3 above the sample 6 to be analyzed.
[0141] For the determination in an analytical and / or sensory manner, the sample 6 (that is to say the active ingredient release system to be analyzed 6, preferably the capsule 6 to be analyzed or the precursor 6 to be analyzed) is located on a sample carrier 7, which in turn is preferably located on a support surface 8. The support surface 8 is generally a plane on which the device 1 of the present invention is also located. In an alternative variant, the sample 6 (that is to say the active ingredient release system to be analyzed, preferably the capsule 6 to be analyzed or the precursor 6 to be analyzed) can also be located directly on the support surface 8. The sample carrier 7 and the support surface 8 can also be part of the device 1.
[0142] The sample carrier 7 or the support surface 8 on which the sample 6 to be analyzed lies is preferably arranged within the basic frame 2 of the device according to the invention.
[0143] The support surface 8 is preferably a pad having a smooth surface, preferably formed of plastic. The support surface 8 is preferably a rubber pad that prevents the sample carrier 7 from sliding during the analysis process.
[0144] The sample carrier 7 may also be a fabric, such as clothing, laundry, etc., formed of cotton, linen, wool, viscose, polyacrylic acid, polyamide, polyester, or other organic or inorganic substrates or surfaces thereof, such as tiles, linoleum, wood, glass, metal, hair, etc., or may be a fiber blanket, for example, in order to test the distribution or adhesion of the active ingredient release system on a specific substrate.
[0145] In an alternative variant in which the sample 6 is located directly on the support surface 8, for example in the case of a floor cleaner with encapsulated active ingredients 6 or precursors 6, the device of the invention for analyzing the active ingredients can be positioned directly above the support surface and analyze the surface of the support surface 8. In this case, the support surface 8 can also be a fabric such as clothing, washing, etc. formed of cotton, linen, wool, viscose fibers, polyacrylic acid, polyamide, polyester, or other organic or inorganic substrates or surfaces thereof such as tiles, linoleum, wood, glass, metal, hair, etc. or can be a fiber carpet.
[0146] According to the first aspect of the present invention, the device for determining an active ingredient or multiple active ingredients from a release system, especially a capsule 6 or a precursor 6 in an analytical and / or sensory manner further comprises a detection device or an analysis device 5 for obtaining the released active ingredient or the released multiple active ingredients in an analytical manner. The detection device or the analysis device 5 is designed to be able to deliver the released active ingredient or the released multiple active ingredients into the detection device 5 via a detection conduit 35.
[0147] The detection device or analysis device 5 is a measuring instrument that can perform qualitative and / or quantitative analysis on the released active ingredients.
[0148] The detection device or analysis device 5 is preferably selected from the group consisting of: gas chromatography (GC), gas chromatography / mass spectrometry (GC / MS), ion mobility spectrometry (IMS), FAIMS (high-field asymmetric waveform ion mobility spectrometry), GC-FAIMS and GC-MS-FAIMS or a combination of the above measuring instruments.
[0149] As the detection device or analysis device 5 , it is preferred to use IMS (ion mobility spectrometry), FAIMS (high-field asymmetric waveform ion mobility spectrometry), GC-FAIMS and GC-MS-FAIMS or a combination of the above-mentioned measuring instruments for analysis.
[0150] Detection device or analytical device is most preferably FAIMS (high field asymmetric waveform ion mobility spectrometry).FAIMS can realize the detection and analysis of volatile chemical substances directly from the gas phase in the air flow or from the liquid or solid sample top.There are two mechanisms to send sample into the FAIMS unit: single sample introduction or continuous sample introduction.In the case of single sample introduction, collect or enrich the gaseous analyte of limited volume, that is to say the released active ingredient in the pre-step by adsorption mode and send it into FAIMS.In the case of continuous sample introduction, gaseous analyte, that is to say the released active ingredient is continuously sent into FAIMS by means of carrier gas.Sampling is preferably carried out continuously, so that the released active ingredient can be measured in real time in an analytical manner.It can be realized that the real-time release is measured in an analytical manner thus, which is particularly advantageous when measuring the release of a fragrance substance mixture or a taste substance mixture.
[0151] In addition, the released active ingredient or the multiple active ingredients released can be combined on the adsorbent, for example, in the Tenax tube, by utilizing the equipment 1 of the present invention, so that it is concentrated and then measured by means of GC-MS (dynamic headspace method). In the dynamic headspace technology, the active ingredient released during measurement or the multiple active ingredients released during measurement are directed to, for example, the Tenax tube or the suitable adsorbent material in the cold trap via a continuous gas flow or an inert gas, for example, produced by FAIMS or formed using an additional external pump. The glass tubule containing adsorbent can be directly combined by CBA in the gas flow, or the active ingredient is first (under an air flow too high for the direct method) directed to a closed container (for example, a plastic bag), so that the active ingredient is subsequently directed to the adsorbent with a smaller air flow. Subsequently, the Tenax tube (adsorbent) or the trap is heated, and the analyte enriched, for example, arrives at FAIMS or is used for the column of gas chromatography.
[0152] In a preferred variant, the detection device or analysis device 5 has an alternative outlet port for an olfactometer and / or an olfactory detection port (ODP) (sniffing port system) 52, with which the released active ingredient can be simultaneously determined in a sensory manner, so that in addition to a qualitative and / or quantitative analysis, a sensory analysis of the active ingredient can also be performed. Such a combination allows a link between analytical and sensory determinations.
[0153] In the device of the present invention, the sniffing port system can be arranged not only before the detection device 5, but also after the detection device 5. When the detection device 5 is a FAIMS or an IMS, it is particularly advantageous to arrange the sniffing port system after the detection device 5, because the FAIMS or the IMS does not destroy the analyte and the analyte is still available at the outlet of the FAIMS or the IMS. In such an arrangement, a correlation can be established particularly well between the measured data of the released active ingredient and the perception score.
[0154] In a most preferred variant of the device of the invention, the FAIMS is combined with a gas chromatograph (GC) and / or a mass spectrometer (MS) and / or an olfactometer and / or an olfactory detection port (ODP) (sniffing port system) (52).
[0155] The activation device 3 of the device according to the first aspect of the present invention includes an activator 31. The activator 31 is preferably formed in the form of an embossing head and is arranged at the lower end of the axis of the activation device 3 and perpendicular to the plane of the support surface 8. The activator 31 is connected to a Z positioning unit 32. The Z positioning unit 32 can realize the lifting and lowering of the activator perpendicular to the sample carrier 7 or perpendicular to the support surface 8. With the help of the Z positioning unit 32, the activator 31 can be moved and positioned on the sample carrier 7 or the support surface 8 perpendicular to the sample carrier 7 or the support surface 8 and thus perpendicular to the sample 6 (that is, perpendicular to the active ingredient release system to be analyzed, preferably the capsule to be analyzed or the precursor 6 to be analyzed).
[0156] The Z positioning unit 32 is a positioning unit that can be used to manually lower the activator 31 or can lower the activator above the sample to be analyzed via an electric drive / motor controlled by the EDV. The positioning unit is preferably a motor that manipulates the coordinates of the sample to be analyzed with the help of the EDV controller and lowers the activator 31 above the sample to be analyzed.
[0157] The activator 31 is configured to apply physical and / or chemical stimulation to the sample to be analyzed 6, that is, the release system 6, preferably the capsule 6 or the precursor 6, so as to open the capsule when the release system is a capsule, or to activate the precursor and release the active ingredients contained therein when the release system is a precursor.
[0158] The physical and / or chemical stimulation is the influence on the release system by pressure, friction, temperature, pH change, UV radiation, ultrasound, microwave or chemical reaction, by means of which the capsule is opened or the precursor is activated. For this purpose, the activator 31 is correspondingly designed as, for example, a friction head, a UV lamp, a pipette module, etc.
[0159] If the release system is a capsule, it can be opened by different opening mechanisms, thereby releasing the capsule contents or active ingredient. In most cases, the release system or capsule is opened by mechanical stress, such as pressure or shear force. Alternative opening mechanisms that can be used to release the active ingredient from the release system or capsule are temperature, pH change, microwaves, light energy such as UV radiation or ultrasound.
[0160] Mechanical pressure and / or friction is preferably applied vertically to the sample 6 by means of the activator 31 in order to thereby break the release system, preferably the capsule, and release the active ingredient contained therein. The mechanical pressure is generated via a pressure sensor 33. The pressure applied to the active ingredient release system, preferably the capsule, can be set via the pressure sensor 33 in order to open the release system, that is to say to burst or rupture it.
[0161] In order to generate friction forces which also cause the active ingredient release system to rupture or burst, the activation device comprises a rotating unit 38. The activator 31 is directly connected to the rotating unit 38 which is driven by a motor. The rotating unit 38 moves the activator 31, for example by concentric, eccentric or equidistant movements. In the concentric movement, the activator performs a rotary circular movement on the sample 6 to be analyzed, wherein the circles have different radii. In the eccentric movement, the activator performs a rotary circular movement outside the center of the circle on the sample 6 to be analyzed. In the equidistant movement, the activator moves back and forth in the X and Y directions on the sample 6 to be analyzed like a slider.
[0162] By one of the above movements, the activator 31 is displaced on the sample to be analyzed 6 and generates a friction force, thereby releasing the active ingredient from the active ingredient release system, preferably a capsule.
[0163] In an alternative variant of the activation device 3, the rotating unit is an oscillating unit 38 which vibrates the activator 31. By vibrating the activator over the sample 6 to be analyzed, frictional forces are generated, thereby releasing the active ingredient from the active ingredient release system, preferably a capsule.
[0164] The activator 31 preferably performs a concentric, eccentric or equidistant movement on the sample 6 to be analyzed.
[0165] The surface of the activator 31 facing the sample 6 to be analyzed can be smooth or rough. In a preferred variant, the activator 31 has a rough surface. Due to the rough surface, the friction of the activator 31 on the release system, preferably the capsule, is enhanced. The surface material of the activator 31 is selected from the group consisting of: Teflon, felt, sponge, towels and other textiles, Molton, glass, metal and resin glass. The preferred surface material of the activator 31 is Teflon. The most preferred is felt because it produces a large friction.
[0166] In an alternative variant, the activator 31 is designed to generate other opening mechanisms to open the release system, preferably the capsule. For example, the activator 31 is configured to generate temperature, UV radiation, magnetic radiation, ultrasound or microwaves, which then open the release system, preferably the capsule, and release the capsule contents.
[0167] If the release system is a precursor or precursor substance, the precursor or precursor substance can be activated by an activator 31 by triggering chemical or physical stimuli such as temperature, oxygen (oxidation), light, enzymes, microorganisms, chemical reactions (such as hydrolysis), pH changes or humidity, thereby releasing active ingredients, preferably fragrance substances.
[0168] In a preferred variant, the released active ingredient is a volatile substance.
[0169] The activation device 3 also comprises a detection conduit 35. The released active ingredient or the released active ingredients, preferably in the gas phase, are collected by means of the detection conduit 35 and conveyed to the detection device 5. In a preferred variant, the activation device is adapted to inhale the active ingredient released from the release system by means of an integrated inhalation mechanism and convey it to the detection device 5.
[0170] Furthermore, in an alternative and preferred design, the activation device 3 comprises at its lower end a collecting container 34 which can surround the sample 6 to be analyzed and the activator 31 when the collecting container is placed on the sample carrier 7 or the support surface 8. The collecting container 34 has a detection duct 35 and a flushing duct 36 for collecting the released active ingredients.
[0171] In order to prevent the released active ingredients, in particular gaseous or volatile active ingredients, such as aroma substances or flavor substances, from escaping from the surface of the sample carrier 7 or the support surface 8 in the area covered by the collecting container 34 without reaching the detection device or the analysis device 5, the collecting container 34 is preferably designed so that it is closed laterally and at its upper end and is open at its lower end and at the end facing the sample to be analyzed. When the activation device 3 is lowered above the sample to be analyzed and supported on the sample carrier 7 or the support surface 8, the collecting container ends in an airtight manner at the covered surface.
[0172] In a preferred variant, the collecting container 34 has a bell shape.
[0173] In order to further prevent the released active ingredients from escaping from the surface of the sample carrier 7 or the supporting surface 8 in the area covered by the collecting container or bell-shaped member 34 without reaching the detection device or analysis device 5, the collecting container or bell-shaped member 34 can be provided with a rounded edge or a sealing component, which can terminate flatly at the supporting surface located below, and the sealing component can make the bell-shaped member close to the covered area in a sealing manner, so that the released active ingredients can only escape through the detection line 35 and can thus be forcibly sent to the detection device or analysis device. For example, the collecting container can have a sealing ring that can be composed of fluoroelastomer.
[0174] The collecting container or bell 34 can be made of a transparent material such as glass or plastic. A transparent collecting container or bell 34 has the advantage that the surface covered by the collecting container or bell 34 can be observed during the opening or activation of the release system, preferably capsule 6 or precursor 6, the release of one or more active ingredients and the analysis.
[0175] The collecting container or bell 34 is arranged on the activation device 3 such that it can be lowered or raised together with the activator 31 by means of the Z-positioning unit 32 perpendicularly to the sample carrier 8 or perpendicularly to the support surface 8 .
[0176] The transparent collecting container 34 further has the following advantageous effect: instead of an activator, the opening or activation of the release system, preferably the capsule 6 or the precursor 6, and the release of one or more active ingredients can alternatively be carried out with the aid of light or by UV radiation by directly passing through the collecting container 34 into the sample to be analyzed.
[0177] In a further embodiment of the device according to the invention, the collecting container or the bell 34 can be lowered or raised perpendicularly to the sample carrier 8 or perpendicularly to the support surface 8 independently of the Z positioning of the activator 31 .
[0178] In an alternative and preferred variant, the activation device 3 comprises a detection duct 35 connected to a collecting container or bell 34. The detection duct 35 is designed so that it conveys the active ingredient released from the release system to the detection device 5. The detection duct is preferably made of metal or of a plastic polymer.
[0179] The released active ingredient to be analyzed is preferably a volatile substance, such as a volatile odorant or flavorant, or a mixture of volatile odorants or flavorants, which is directly guided to the detection device 5 and analyzed in the detection device. In a preferred variant, the volatile substance is sucked in and sent to the detection device 5 by means of a detection conduit 35 via an integrated suction mechanism. In other cases and in an alternative variant, the released active ingredient reaches the detection device or analysis device 5 by means of an inert gas (such as nitrogen or helium). For this purpose, an inert gas is introduced into the collection container via a conduit connected to the collection container or bell 34, thereby pushing out the volatile substance and guiding it to the detection device 5.
[0180] Optionally, the activation device 3 comprises a flushing conduit 36 connected to the collecting container or bell 34. The flushing conduit 36 is adapted to be used to send a flushing gas or a flushing liquid into the system after the opening process, the release process and the analysis process are completed, so as to flush the collecting container or bell 34 and / or the detection conduit 35. By flushing, traces of active ingredients are removed, so that the system can be used for the next analysis process without contamination. The flushing gas is preferably selected from air, nitrogen or helium. It is preferred to use water or a polar or non-polar solvent as a flushing liquid, preferably ethanol, acetone, isopropanol, heptane or an aqueous detergent solution, and the aqueous detergent solution is used in combination with another final flushing step when appropriate. In other cases, wait between two analysis processes until the residues of the volatile active ingredient have evaporated.
[0181] Residual flushing gas or flushing liquid, residual active ingredients of the encapsulated active ingredients and other sample residues can be blown away from the activation device 3, preferably from the collecting container 34 and / or from the activator 31, by means of a ventilator 39, which is optionally a component of the activation device 3.
[0182] The device according to the first aspect of the invention further comprises an EDV system 51 with suitable software for controlling and positioning the device 1 and for analyzing and storing the measurement results.
[0183] In a preferred variant, the X / Y positioning unit (4) of the device according to the first aspect of the invention comprises a positioning laser (43). The positioning laser (43) is part of the positioning unit of the EDV system or computer 51 for controlling the X-axis 21, Y-axis 22 and activating the movement of the device 3.
[0184] The sample carrier 7 preferably has a grid formed by evenly spaced horizontal and vertical lines, by which a grid with a uniform sample area is created. The sample area forms the (surface) surface onto which the sample to be analyzed is loaded or positioned.
[0185] In order to position and move the activation device 3 above the sample carrier 7, the measuring start and end points of the sample area and the number of horizontal and vertical sample areas on the sample carrier 7 are required to adjust (train) the device 1. These positions are acquired by the position laser 41 and stored in the device 1 via the EDV system. Starting from the acquired and stored measuring start and end points of the sample area (defined by means of the position laser), the activation device 3 can be positioned exactly above the sample area to be analyzed and can leave the sample area.
[0186] At the beginning of a measurement or a measurement sequence or before the breaking process, release process and analysis process, the X-axis 21, the Y-axis 22 and the activation device 3 are moved to the "zero point" of the base frame 2, that is to say the starting point. Once the "zero point" is reached, a signal is sent to the computer. Based on this "zero" point, the starting point and the end point can be specified for each coordinate in combination with the movement of the positioning unit. Through these coordinates related to the number of measurements in the horizontal and vertical direction, a coordinate can be calculated for each measuring point and moved to the coordinates accordingly and automatically.
[0187] The device 1 for analytically and / or sensory determination of a release system and / or an encapsulated active ingredient according to the first aspect of the invention provides a system that can perform an objective and standardized analytical method. This in turn makes it possible to draw conclusions qualitatively and / or quantitatively about the release of one or more active ingredients, such as the concentration of the released active ingredient, the release rate or the release profile, and / or draw conclusions about the properties of the active ingredient release system, preferably the capsule or the precursor, such as the mechanical stability, the breaking strength and the hysteresis behavior of the capsule after a certain storage period.
[0188] Furthermore, the device 1 according to the first aspect of the invention is fully automatically operated. A fully automatically operated device 1 has the following advantages, for example, the device allows the following analysis parameters to be set accurately: pressure, length of time for pressure-free measurement, target for pressure in the absence of friction, detection time of friction process and friction-free, rotation speed, rotation duration or flushing time. With the aid of the device 1 according to the invention, determinations can be carried out simultaneously in an analytical and / or sensory manner, whereby a correlation of the obtained measurement results can be obtained. Furthermore, the device 1 according to the invention allows the analysis of a real-time analysis of the release of one or more active ingredients from the release system used according to the invention.
[0189] Furthermore, the device 1 according to the invention makes it possible for the first time to reproducibly and objectively determine the bursting behavior of encapsulated active ingredients (e.g. flavoring substances or aromatic substances) analytically and / or sensorially. This allows the screening of new capsule technologies and the development of capsules with optimal bursting behavior without a huge expenditure of time and personnel and without adversely affecting the subjectivity of the sensory panel.
[0190] In a second aspect, the present invention is therefore directed to a method for analytically and / or sensorily determining the release of an active ingredient or active ingredients from a release system, preferably from a capsule or a precursor.
[0191] In the context of the present invention, a release system 6 is understood to be a solid preparation, such as microparticles or capsules 6 or precursors 6 or precursor substances, as already defined above, comprising one or more active ingredients.
[0192] The capsule 6 analyzed by the method of the present invention is preferably a capsule selected from the group consisting of hard capsules (hard shell capsules), soft capsules (soft shell capsules), macrocapsules, microcapsules, capsule slurries and capsule emulsions.
[0193] The active ingredient contained in the release system, preferably the active ingredient contained in the capsule or the active ingredient released from the precursor is a solid, liquid or gaseous substance.
[0194] The active ingredient of the release system is preferably a volatile substance that can volatilize at room temperature and is preferably selected from the group consisting of: fragrance substances, flavor substances, perfume oils, fragrance substance mixtures, flavor substance mixtures, aromatic substances, plant extracts, essential oils, cosmetic active ingredients, cooling active ingredients and pharmaceutical active ingredients. For the contents of various active ingredients, please refer to the above description.
[0195] In a first step of the method according to the invention, a sample 6 , ie a release system 6 to be analyzed which comprises one active ingredient or several active ingredients, is provided on a sample carrier 7 which is located on a support surface 8 .
[0196] The sample carrier 7 may also be a fabric, such as clothing, laundry, etc., formed of cotton, linen, wool, viscose, polyacrylic acid, polyamide, polyester, or other organic or inorganic substrates or surfaces thereof, such as tiles, linoleum, wood, glass, metal, hair, etc., or may be a fiber blanket, for example, in order to test the distribution or adhesion of the active ingredient release system on a specific substrate.
[0197] As an alternative thereto, the release system 6 , preferably the capsule 6 or the precursor 6 , is located directly on the support surface 8 in the method according to the invention.
[0198] In an alternative variant in which the sample 6 is located directly on the support surface 8 , for example in the case of a floor cleaner with encapsulated active ingredients 6 or precursors 6 , the device according to the invention can be positioned directly above the support surface and analyze the surface of the support surface 8 directly.
[0199] The amount of release system 6, preferably capsules 6 or precursors 6, applied to the sample carrier 7 is variable and depends on the material and diameter of the friction head, the application of the capsules or precursors and the active ingredient content in the capsules or precursors. The application to the sample carrier is preferably carried out in the form of a capsule slurry, preferably at a concentration close to that used, for example taking into account the concentration in standard washing powder water in a washing machine and taking into account the average adhesion of the capsules to the laundry during the washing process. The amount applied is 0.1 mg to 2.0 mg of capsules or precursors per measurement area or sample area on the sample carrier, more preferably still 0.3 to 1.8 mg and most preferably 0.5 to 1.0 mg of capsules or precursors per measurement area or sample area.
[0200] As an alternative thereto, the amount of release system can be adapted to the application, for example when the adhesion of the release system to the textile is determined after a machine washing process.
[0201] The sample carrier 7 preferably has a grid formed by evenly spaced horizontal and vertical lines, thereby creating a grid formed by uniform measurement areas or sample areas. The sample to be analyzed 6, that is to say the release system 6 to be analyzed, preferably the capsule 6 or the precursor 6, is applied to the sample carrier 7 within a specific measurement area or sample area with individual coordinates. By training the device of the invention (via a laser) and giving the rows and columns before the start of the measurement, the grid coordinates are calculated and manipulated independently by the EDV. Thus, the activation device 3 can be controlled to the corresponding sample area on which the sample to be analyzed has been applied or positioned.
[0202] In the next step of the method according to the invention, the activation device 3 with the activator 31 is positioned above the release system 6, in particular the capsule 6 or the precursor 6. The movement and positioning of the activation device 3 with the activator 31 is carried out horizontally and in the X and Y directions relative to the sample carrier 7 or the support surface 8 on which the sample to be analyzed is located, via the X-axis 21 and the Y-axis 22 or via the X-positioning unit / X-positioning drive 41 and the Y-positioning unit / Y-positioning drive.
[0203] In another step of the method according to the second aspect of the invention, the activation device 3 is lowered so that the activator 31 is at a distance from the release system 6, in particular the capsule or the precursor, or slightly touches the release system 6. This is done depending on the stimulus used to open or activate the release system. When opening or activating by means of pressure and / or friction, the activator 31 touches the release system, while when opening or activating by means of UV radiation, it can be at a distance from the release system.
[0204] Next, in the method of the present invention, the active ingredient or the multiple active ingredients are released from the release system 6, preferably the capsule 6 or the precursor 6 by means of an activator. The release of the active ingredient or the multiple active ingredients is carried out by physical or chemical stimulation. If the release system is a capsule, the release of the active ingredient is carried out by opening the capsule by means of pressure, friction, temperature, pH change, UV radiation, microwaves and ultrasound. If the release system 6 is a precursor 6, the release of the active ingredient from the precursor material is carried out by chemical reaction, temperature, humidity, pH change, oxygen (oxidation), light such as UV radiation, enzymes and microorganisms.
[0205] In a preferred variant of the method, the active ingredient or ingredients are released from the capsule by means of an activator by pressure on the sample to be analyzed 6 and / or friction on the sample to be analyzed 6. Depending on the capsule material, for example in the case of thin capsule walls or unstable capsule materials, in an alternative variant of the method according to the invention, the capsule is broken only by applying pressure and without friction.
[0206] The mechanical pressure is generated via the pressure sensor 33. The pressure applied to the active ingredient release system, preferably the capsule, can be set via the pressure sensor 33 so that the release system bursts or breaks. The pressure in the method of the present invention acting on the active ingredient release system (preferably the capsule) to destroy it and release the active ingredient is ≥0Pa. It can be verified that a pressure of 0Pa, that is to say when the activator 31 is simply moved close to the sample 6 to be analyzed, is sufficient to break the first capsule. Preferably, the method is performed on the active ingredient release system, preferably the capsule or the sample carrier 7 at a pressure in the range of 1000Pa to 30000Pa, and more preferably at a pressure in the range of 2500Pa to 25000Pa. These values preferably relate to a radius of 2cm. The above-mentioned minimum and maximum pressures are adapted by changing the radius of the activator or selecting the friction head material.
[0207] In order to generate friction forces which also cause the active ingredient release system to rupture or burst, the activation device comprises a rotating unit 38. The activator 31 is directly connected to the rotating unit 38 which is driven by a motor. The rotating unit 38 moves the activator 31, for example by concentric, eccentric or equidistant movements. In the concentric movement, the activator performs a rotary circular movement on the sample 6 to be analyzed, wherein the circles have different radii. In the eccentric movement, the activator performs a rotary circular movement outside the center of the circle on the sample 6 to be analyzed. In the equidistant movement, the activator moves back and forth in the X and Y directions on the sample 6 to be analyzed like a slider.
[0208] By one of these movements, the activator 31 is displaced on the sample to be analyzed 6 and generates friction forces, thereby releasing the active ingredient from the release system, preferably the capsule.
[0209] In an alternative variant, the activator 31 is an oscillating unit 38 which vibrates the activator 31. By vibrating the activator over the sample 6 to be analyzed, frictional forces are generated, thereby releasing the active ingredient from the release system, preferably a capsule.
[0210] In a further alternative variant, the direction of rotation of the activator can be changed at shorter time intervals during the measurement, as a result of which the active ingredient is released from the active ingredient release system, preferably the capsule.
[0211] In the method of the present invention, the active ingredient is released from the release system 6, in particular from the capsule 6, with the aid of an activator 31, while touching the encapsulated active ingredient 6 and / or the sample carrier 7 at a rotational speed of 0 rpm of the activator 31, preferably at a rotational speed of 50 to 1,000 rpm and still more preferably at a rotational speed of 200 to 1,000 rpm.
[0212] The friction time in the method of the present invention is variable. The friction time is preferably 0 to 30 seconds.
[0213] The method parameters pressure and friction have the greatest influence on the bursting of the capsules. Advantageously, these two method parameters can be set accurately with the method according to the invention and in an automated manner. Due to the different settings of the method parameters, capsules of different sizes and capsule walls of different strengths can also be broken. In addition, for example, increasing the pressure can release the active ingredient from the release system more quickly, so that a stronger strength can be measured in the subsequent analytical and / or sensory determination. Conversely, the pressure applied in order to burst the capsule can be regarded as a parameter of the breaking strength and thus as a parameter of the capsule stability.
[0214] In a preferred variant, the released active ingredient is a volatile substance.
[0215] In another step of the method according to the invention, the released active ingredient or the released active ingredients, preferably present in the gas phase, are collected by means of a detection conduit 35 and conveyed to a detection device 5. In a preferred variant, in the method according to the invention, the active ingredient released from the release system is sucked in by means of an integrated suction mechanism, preferably a pump of FAIMS, and conveyed to the detection device 5.
[0216] In a preferred variant of the method of the present invention, in order to prevent the released active ingredients, especially gaseous or volatile active ingredients, such as aroma substances or flavor substances, from escaping when being measured in an analytical and / or sensory manner, the surface of the sample carrier 7 or the support surface 8 on which the sample is located is covered with a collecting container 34, which preferably has a bell-shaped shape and is arranged at the lower end of the activator 31. For this purpose, the collecting container 34 is preferably designed so that it is closed laterally and at its upper end and is open at its lower end and at the end facing the sample to be analyzed. When the activation device 3 is lowered above the sample to be analyzed and supported on the sample carrier 7 or the support surface 8, the collecting container ends at the covered surface in an airtight manner. This prevents the released active ingredients, especially volatile active ingredients, such as aroma substances or flavor substances, from escaping from the surface of the sample carrier 7 or the support surface 8 in the area covered by the collecting container 34 without reaching the detection device or the analysis device 5.
[0217] In an optional variant, the released active ingredient can be sucked by means of a pump from the collecting container or bell into the detection device or analysis device 5. This has the advantage that the released active ingredient can be detected after a few seconds.
[0218] In a further step of the method according to the invention, the active ingredient released from the release system, preferably the capsule or the precursor, is fed to a detection device or an analysis device 5 for analytically and / or sensorially determining the released active ingredient.
[0219] In a further step of the method according to the invention, the active ingredient released from the release system is determined analytically and / or sensorially by means of a detection device or analysis device 5 .
[0220] Acquiring and / or determining analytically is understood to mean analyzing the active ingredient released from the release system 6, in particular from the capsule 6 or precursor 6, sensorily, qualitatively (identification of the active ingredient) and / or quantitatively (amount of the active ingredient). Advantageously, the method according to the invention can be used to analyze the active ingredients of the release system, for example encapsulated active ingredients, by type and amount.
[0221] The detection device or analysis device 5 is a measuring instrument that can perform qualitative and / or quantitative analysis on the released active ingredients.
[0222] In order to qualitatively and / or quantitatively analyze the released active ingredients, it is preferred to use a detection device or analysis device 5 preferably selected from the group consisting of: gas chromatography (GC), gas chromatography / mass spectrometry (GC / MS), ion mobility spectrometry (IMS), FAIMS (high-field asymmetric waveform ion mobility spectrometry), GC-FAIMS and GC-MS-FAIMS or a combination of the above-mentioned measuring instruments.
[0223] As the detection device or analysis device 5 , it is preferred to use IMS (ion mobility spectrometry), FAIMS (high-field asymmetric waveform ion mobility spectrometry), GC-FAIMS and GC-MS-FAIMS or a combination of the above-mentioned measuring instruments for analysis.
[0224] In the method of the present invention, the released active ingredient is most preferably measured analytically by means of FAIMS (high field asymmetric waveform ion mobility spectrometry).FAIMS can realize the detection and analysis of volatile chemical substances directly from the gas phase in the airflow or from the liquid or solid sample.There are two mechanisms to send the sample into the FAIMS unit: single injection or continuous injection.In the case of single injection, the gaseous analyte of the limited volume, that is to say the released active ingredient is collected by adsorption mode in the preceding step and sent to FAIMS.In the case of continuous injection, the gaseous analyte, that is to say the released active ingredient is continuously sent to FAIMS by means of carrier gas (for example purified air or argon).Injection is preferably carried out continuously, so that the released active ingredient can be measured analytically in real time.It can be realized that the real-time release is measured analytically, which is particularly advantageous when measuring the release of a fragrance substance mixture or a taste substance mixture.
[0225] In an alternative variant of the inventive method, the released active ingredient is for example attached to an adsorbent in a Tenax pipe, so that it is concentrated and measured by means of GC-MS subsequently (dynamic headspace method). In the dynamic headspace technique, the active ingredient released during measurement or the multiple active ingredients released during measurement are directed to a suitable adsorbent material in, for example, the Tenax pipe or in a cold trap via a continuous gas flow or an inert gas such as produced by FAIMS or formed using an additional external pump. The glass tubule containing adsorbent can be directly combined by CBA in the gas flow, or the active ingredient is first (under an air flow too high for the direct method) directed to a closed container (for example a plastic bag), so that the active ingredient is directed to the adsorbent with less air flow subsequently. Tenax pipe (adsorbent) or trap are heated subsequently, and the analyte of the enrichment for example arrives at FAIMS or is used for the post of gas chromatography.
[0226] In a preferred variant of the method according to the invention, in addition to the qualitative and quantitative determination of the active ingredient released, the active ingredient released is also determined sensorially by means of an olfactometer and / or an olfactory detection port (ODP) (sniffing port system) (52) connected via an alternative outlet port to the detection device or analysis device 5. Such a combination allows a correlation between analytical and sensorial determinations.
[0227] In the device of the present invention, the sniffing port system can be arranged not only before the detection device 5, but also after the detection device 5. When the detection device 5 is a FAIMS or an IMS, it is particularly advantageous to arrange the sniffing port system after the detection device 5, because the FAIMS or the IMS does not destroy the analyte and the analyte is still available at the outlet of the FAIMS or the IMS. In such an arrangement, a correlation can be established particularly well between the measured data of the released active ingredient and the perception score.
[0228] The obtained measurement results are fed to an EDV system 51 with suitable software and are analyzed and stored with the aid of the software.
[0229] In the final step of the method according to the invention, the device 1 is reset, wherein the reset of the device 1 comprises the following steps: firstly, the activation device 3 is raised by means of the Z positioning unit 32 .
[0230] The method of the present invention optionally includes the following steps, wherein the activator 31 and / or the detection conduit 35 and / or the detection device are flushed with a flushing gas or a flushing liquid after the opening process, the release process and the analysis process are completed. By flushing, the residues of the released active ingredients or other sample residues are removed, so that the system can be used for the next analysis process without pollution. The flushing gas is preferably selected from air, nitrogen or helium. It is preferred to use water or a polar or non-polar solvent as the flushing liquid, preferably ethanol, acetone, isopropanol, heptane or a detergent aqueous solution, and the detergent aqueous solution is combined with another final flushing step when appropriate. In other cases, wait between two analysis processes until the residues of the released active ingredients have evaporated.
[0231] In the method of the present invention, residual flushing gas or flushing liquid, residual active ingredients of the encapsulated active ingredients and other sample residues can be blown away from the activation device 3, preferably from the activator 31 and / or from the collection container 34, using a ventilator 39 (optionally a component of the activation device 3).
[0232] A schematic overview of the steps of the method of the present invention is given in Figure 5 Shown in.
[0233] The method according to the second aspect of the invention can be used to analyze the active ingredient from the release system, preferably the capsule or the precursor objectively and under standardized conditions, that is, when the defined method parameters are set. The analytical method of the present invention can be used to break the active ingredient release system, preferably the capsule or the precursor under well-defined conditions (such as pressure), that is, in a standardized and controlled manner, and simultaneously analyze the capsule contents quantitatively and / or qualitatively. This can achieve a standardized, standardized and reproducible analytical method, wherein the applicable conditions and the flow of the analytical method are fixed, so that the same results should be expected under the same preconditions. This can also be achieved, so that the measurement results of different capsule samples or precursors can be compared with each other. Such determinations performed in an analytical and / or sensory manner under reproducible release conditions were previously unknown.
[0234] According to the method of the present invention, the bursting behavior of the encapsulated active ingredient can be determined reproducibly and objectively in an analytical and / or sensory manner, thereby enabling the screening of new capsule technologies and the development of capsules with optimal bursting behavior without a huge expenditure of time and personnel and without adversely affecting the subjectivity of the sensory panel.
[0235] In addition, the method according to the invention makes it possible for the first time to continuously measure the release of one or more active ingredients from a capsule or from a precursor, wherein the time curve of the release can be recorded directly (ie in parallel with the release). Such online measurements are performed, for example, in Figure 6 Reappear in.
[0236] Figure 6 The curve shows the continuous measurement of capsule bursting of capsules containing perfume oil. The capsules are multilayer capsules with a core of liquid perfume oil. Measuring parameters: rubbing at 1.0 N for 10 s at 60 rpm; post-rubbing time 30 s.
[0237] In particular, after the friction head is raised, a bursting of the capsule (capsule breakage) and the release of the perfume oil can be seen. The maximum of the release curve is reproducible and can be used to compare different capsules.
[0238] The method according to the invention can also realize continuous operation, wherein a plurality of samples can be analyzed successively, for example under the same method parameters. The analysis values can thus be directly compared with each other. In addition, through the combination of the detection device 5 with an alternative outlet port for an olfactometer and / or an olfactory detection port (ODP) (sniffing port system) 52, an improved receptive evaluation and comparison of different samples can be carried out by a reproducible release method.
[0239] Furthermore, the analytical and receptive measurement results thus obtained can be correlated with one another.
[0240] Due to the above advantages, the device of the present invention and the method of the present invention are preferably suitable for analytically and / or sensorily determining the release of active ingredients from the release system 6, preferably from the capsule 6 or precursor 6, in order to thereby analyze the composition of the active ingredients according to type and amount.
[0241] In particular in the development and production of new capsules, the method according to the invention can also be used to analyze the mechanical stability and fracture behavior of different capsule materials. Furthermore, the method according to the invention allows the hysteresis behavior of the capsules to be analyzed, preferably after the capsules have been stored for a certain period of time.
[0242] The method according to the invention also enables the release of various active ingredients, for example different odorants or flavor substances or fragrance mixtures or aroma mixtures, from a release system, preferably from a capsule or precursor.
[0243] The method according to the invention furthermore allows the distribution and adhesion of microcapsules on surfaces to be analysed, for example the distribution and adhesion of microcapsules containing fragrance substances after washing and drying of textiles.
[0244] The method of the invention can also enable the analysis of the affinity of an active ingredient or multiple active ingredients on a substrate after release from a release system 6 , in particular a capsule 6 or a precursor 6 ;
[0245] In addition, the method of the present invention can be used to analyze the influence of physical or chemical factors such as temperature, light, UV radiation, pH value on the mechanical stability and breaking strength of the release system, especially the capsule or precursor 6 and / or on the release of one or more active ingredients from the release system 6, especially the capsule 6 or the precursor 6.
[0246] The method according to the invention can also be used to analytically determine the release of an active ingredient or active ingredients during the development and production of a delivery system 6 and to determine the properties of a delivery system 6 , in particular a capsule 6 or a precursor 6 .
[0247] Therefore, in a final aspect, the present invention relates to the use of the device according to the invention and the method according to the invention for analytically and / or sensory determination of the amount of a substance released from a release system (6), in particular a capsule (6) or a precursor (6).
[0248] Release of an active ingredient or multiple active ingredients, in particular determination of the concentration, release rate or release profile;
[0249] - for determining the properties of a release system (6), in particular a capsule (6) or a precursor (6), in particular the mechanical stability, breaking strength and hysteresis behavior, in particular the mechanical stability, breaking strength or hysteresis behavior of capsules (6) formed from different capsule materials and different active ingredients;
[0250] - for analyzing the distribution and adhesion of a release system (6), in particular a capsule (6) or a precursor (6), on a substrate, in particular after washing and drying of textiles;
[0251] - for analyzing the affinity of an active ingredient or multiple active ingredients on a substrate after release from the release system 6, in particular the capsule 6 or the precursor 6;
[0252] - for analyzing the influence of physical or chemical factors such as temperature, light, UV radiation, pH value on the mechanical stability and breaking strength of the release system, in particular the capsule or precursor 6 and / or on the release of one or more active ingredients from the release system 6, in particular the capsule 6 or the precursor 6; and
[0253] For analytically determining the release of an active ingredient or several active ingredients and for determining the properties of a release system 6 , in particular a capsule 6 or a precursor 6 , during the development and production of the release system 6 .
[0254] Example 1: Comparison of flavor release from different capsule technologies
[0255] Comparison of analytical bursting behavior of different capsule types. Types A to D are core / shell perfume oil capsules based on methylformamide and differ in their wall thickness (wall thickness decreases from A to D). All capsule types are loaded with the same perfume oil at the same dosage. Measurements are performed at 2.5 N for 15 s; friction: 100 rpm.
[0256] The results of the maximum burst strength are Figure 7 The burst strength is highest in the case of capsule type D, which has the smallest wall thickness.
[0257] Reference numerals list:
[0258] 1 Equipment
[0259] 2 Basic Framework
[0260] 21 X-axis
[0261] 22 Y-axis
[0262] 3 Activate the device
[0263] 31 Activator
[0264] 32 Z positioning unit
[0265] 33. Pressure sensor
[0266] 34 Collection container / bell
[0267] 35 Detection catheter
[0268] 36 Flushing catheter
[0269] 37 Flushing pump
[0270] 38 Rotation Unit
[0271] 39 Ventilator
[0272] 4 X / Y positioning units
[0273] 41 X positioning unit / X positioning drive
[0274] 42 Y positioning unit / Y positioning driver
[0275] 43 Positioning laser
[0276] 5. Detection device / analysis device
[0277] 51 EDV system
[0278] 52 Sniffing Port System
[0279] 6 Sample / release system / capsule / precursor
[0280] 7 Sample carrier
[0281] 8 Support surface
Claims
1. A device (1) suitable for determining the release of an active ingredient or multiple active ingredients from a release system (6) in an analytical and / or sensory manner and / or suitable for determining the properties of a release system (6), wherein the release system is located on a sample carrier (7) or a support surface (8), the device comprising: (a) Basic framework (2); (b) an activation device (3) connected to the base frame (2) and adapted to open or activate the release system (6) and release the active ingredient; as well as (c) a detection device (5) adapted for analytically determining the released active ingredient and designed to be able to deliver the released active ingredient or the released active ingredients to the detection device (5), The activation device (3) comprises: (i) an activator (31), which is connected to a Z positioning unit (32) and can be moved vertically to the support surface (8) via the Z positioning unit (32) and is designed to apply a physical or chemical stimulus to the release system (6) on the sample carrier (7) in order to release the active ingredient or the active ingredients; (ii) a detection conduit (35) adapted to collect the released active ingredient or the released active ingredients and guide them to the detection device (5); and (iii) optionally a flushing conduit (36) connected to the detection conduit (35) and adapted to deliver a flushing gas or a flushing liquid into the detection conduit (35).
2. The device according to claim 1, wherein the release system (6) is a capsule or a precursor.
3. The device according to claim 1 or 2, wherein The release system (6) is a capsule, and the physical or chemical stimulus applied to the capsule is selected from the group consisting of: pressure, friction, temperature, pH change, UV radiation, microwave and ultrasound, or the release system (6) is a precursor, and the physical or chemical stimulus applied to the precursor is selected from the group consisting of: chemical reaction, temperature, humidity, pH change, oxygen (oxidation), light, enzyme and microorganism.
4. The device according to claim 1 or 2, wherein the activator (31) comprises a collecting container (34), which can surround the release system (6) and the activator (31) when the collecting container is supported on the sample carrier (7) or the supporting surface (8).
5. The device according to claim 1 or 2, wherein the activator (31) has a rough surface.
6. Device according to claim 1 or 2, wherein the activation device (3) has a rotation unit (38) which triggers a concentric, eccentric or equidistant movement at the activator (31).
7. The device according to claim 1 or 2, wherein the device further comprises: At least one X positioning unit (41) and / or Y positioning unit (42) which is connected to the base frame (2) and is adapted to move the activation device (3) relative to the sample carrier.
8. Apparatus according to claim 7, wherein the X-positioning unit and / or the Y-positioning unit comprises a positioning laser (43).
9. A method for analytically and / or sensorily determining the release of an active ingredient or multiple active ingredients from a release system (6), the method comprising the following steps: (i) providing a release system (6) on a sample carrier (7) or a support surface (8), wherein the release system comprises one active ingredient or multiple active ingredients; (ii) positioning an activation device (3) with an activator (31) above the release system (6); (iii) lowering the activation device (3); (iv) releasing the active ingredient or the active ingredients from the release system (6) with the aid of the activator (31); (v) collecting the released active ingredient or the released active ingredients by means of a detection conduit (35) and sending them to a detection device (5); and (vi) determining the active ingredient or the active ingredients released from the delivery system (6) by analytical and / or sensory means; and / or Determining the properties of the release system (6); and / or Analyzing the distribution and attachment of the release system (6) on the substrate; and / or analyzing the affinity of the active ingredient or ingredients on the substrate after release from the delivery system (6); and / or Analyzing the influence of physical or chemical factors on the mechanical stability and breaking strength of a release system (6) and / or on the release of one or more active ingredients from a release system (6); and / or determining the release of one or more active ingredients in an analytical manner and determining the characteristics of a release system (6) during the development and preparation of a release system (6).
10. The method according to claim 9, wherein the delivery system (6) is a capsule or a precursor.
11. The method according to claim 9 or 10, wherein the determining of the active ingredient or multiple active ingredients released from the release system (6) by analytical and / or sensory means comprises determining the concentration, release rate or release characteristic curve of the active ingredient or multiple active ingredients released from the release system (6) by analytical and / or sensory means.
12. The method according to claim 9 or 10, wherein said determining the properties of the release system (6) comprises determining the mechanical stability, breaking strength and hysteresis behavior of the release system (6).
13. The method according to claim 9 or 10, wherein the release system (6) is a capsule, and the determining the properties of the release system (6) comprises determining the mechanical stability, breaking strength or hysteresis behavior of capsules formed from different capsule materials and different active ingredients.
14. The method according to claim 9 or 10, wherein analyzing the distribution and adhesion of the release system (6) on the substrate comprises analyzing the distribution and adhesion of the release system (6) on the substrate after washing and drying the textile.
15. The method of claim 9 or 10, wherein the physical or chemical factors include temperature, light, UV radiation and pH.
16. The method according to claim 9 or 10, wherein the following steps are performed after step (vi): (vii) resetting the device, wherein resetting the device comprises one or more of the following steps: (a) raising the activation device (3); and optionally (β) flushing the activator (31) and / or the detection conduit (35) and / or the detection device (5) with a flushing gas or a flushing liquid; and optionally (γ) Blowing off the residues of the released active ingredient or the released active ingredients and / or other sample residues from the activation device (3).
17. The method according to claim 16, wherein the step (γ) comprises blowing off the residues of the released active ingredient or the released multiple active ingredients and / or other sample residues from the activation device (3) by means of a ventilator (39).
18. The method according to claim 16, wherein the step (γ) comprises blowing off the residues of the released active ingredient or the released multiple active ingredients and / or other sample residues from the activator (31).
19. The method according to claim 9 or 10, wherein the release of the active ingredient or the active ingredients by means of the activator (31) is performed by physical or chemical stimulation.
20. The method according to claim 19, wherein the release system (6) is a capsule, and the physical or chemical stimulus applied to the capsule is selected from the group consisting of: pressure, friction, temperature, pH change, UV radiation, microwaves and ultrasound, or the release system (6) is a precursor, and the physical or chemical stimulus applied to the precursor is selected from the group consisting of: chemical reaction, temperature, humidity, pH change, oxygen (oxidation), light, enzymes and microorganisms.
21. The method according to claim 9 or 10, wherein the release of the active ingredient or the plurality of active ingredients by means of the activator (31) is carried out at a pressure ranging from 0 Pa to 30,000 Pa.
22. The method according to claim 9 or 10, wherein the release of the active ingredient or the plurality of active ingredients by means of the activator (31) is carried out under a pressure of 1000 Pa to 30000 Pa.
23. A method according to claim 9 or 10, wherein the active ingredient or the multiple active ingredients are released by means of the activator (31) at a rotation speed of the activator (31) ranging from 0 rpm to 1,000 rpm while touching the release system (6) and / or the sample carrier (7).
24. A method according to claim 9 or 10, wherein the active ingredient or the multiple active ingredients are released with the aid of the activator (31) at a rotation speed of 50 to 1,000 revolutions per minute of the activator (31) while touching the release system (6) and / or the sample carrier (7).
25. The method according to claim 9 or 10, wherein the release system (6) is selected from the group consisting of hard shell capsules, soft shell capsules, macrocapsules, microcapsules, capsule slurries and capsule emulsions.
26. The method according to claim 9 or 10, wherein the encapsulated active ingredient is selected from the group consisting of: fragrance substances, flavor substances, perfume oils, fragrance substance mixtures, flavor substance mixtures, aromatic substances, plant extracts, essential oils, cosmetic active ingredients, cooling active ingredients, pharmaceutical active ingredients.
27. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to determine the release of one or more active ingredients from a release system (6) in an analytical and / or sensory manner.
28. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to determine the concentration, release rate or release characteristic curve of one or more active ingredients released from a release system (6) in an analytical and / or sensory manner.
29. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to determine the properties of the release system (6).
30. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, For determining the mechanical stability, breaking strength and hysteresis behavior of release systems (6).
31. The use according to any one of claims 27 to 30, wherein the release system (6) is a capsule or a precursor.
32. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, The release system (6) is a capsule, and the use is for determining the mechanical stability, breaking strength or hysteresis behavior of capsules formed from different capsule materials and different active ingredients.
33. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to analyze the distribution and adhesion of the release system (6) on the substrate.
34. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to analyze the distribution and adhesion of release systems (6) on substrates after washing and drying of textiles.
35. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to analyze the affinity of an active ingredient or multiple active ingredients to a substrate after release from the delivery system (6).
36. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, Used to analyze the influence of physical or chemical factors on the mechanical stability and breaking strength of the release system (6) and / or on the release of one or more active ingredients from the release system (6).
37. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, For analyzing the influence of temperature, light, UV radiation and pH value on the mechanical stability and breaking strength of a delivery system (6) and / or on the release of one or more active ingredients from a delivery system (6).
38. Use of the device according to any one of claims 1 to 8 or the method according to any one of claims 9 to 26, It is used to determine the release of one or more active ingredients in an analytical manner and to determine the properties of a delivery system (6) during its development and preparation.
39. Use according to any one of claims 33 to 38, wherein the release system (6) is a capsule or a precursor.
Citation Information
Patent Citations
Methods, compositions and articles for olfactory-active substances
CN103037907A
Microcapsules containing a hydrophobic, volatile substance
EP0142242A1
Sealed sample injector for gas chromatography
US3002387A
Device for checking pharmaceutical products, in particular hard gelatin capsules
WO2012139811A1
