Technological process for the production of dry myrtle and laurel extract

Abstract

Process for producing and obtaining dietary supplements based on the symbiotic action of myrtle (Myrtus communis L.) and laurel (Laurus nobilis L.) extracts) intended for the modulation of intestinal microflora, which takes place in several steps: first, grinding with a cryogenic mill in liquid nitrogen to a particle size of 40 to 50 μm, using a 30% aqueous ethanol solution as the extraction solvent; then, extraction of targeted bioactive molecules (phenolic compounds) from laurel and myrtle is carried out using microwaves (MAE); the produced extracts are then evaporated in a vacuum concentrator, where they are standardized to a total phenol concentration of 25 g / L; after that, the standardized extracts are mixed in a volume ratio of myrtle:laurel=3:1; then, spray drying of the prepared mixture of myrtle and laurel extracts is carried out at a temperature of 180 °C, with the addition of a combination of carriers β-cyclodextrin and maltodextrin (1:1), in a sample to carrier ratio of 1:2 to a final dry matter content of at least 95%; Finally, the resulting powder is packaged into capsules, and the capsules are packaged into glass vials.

Description

DESCRIPTION OF THE INVENTION Technical field The broader technical field to which this invention belongs is the food and pharmaceutical industry, and the narrower field is biotechnical sciences, namely extraction and encapsulation. This invention relates to a technological process for the production and composition of food supplements based on symbiotic action extract of myrtle (Myrtus communis L.) and laurel (Laurus nobilis L.) intended for modulation of intestinal microflora. The result is an optimized extraction and encapsulation procedure of myrtle and laurel extract that enables optimal utilization bioactive molecules-phenolic compounds and their stabilization and improved bioavailability. According to the International Classification of Patents, the invention belongs to the following areas of technology: A23L 33 / 105 - Extracts of plants, their artificial duplicates or their derivatives A 61 K 35 / 00 - Medical preparations containing substances of unspecified composition or producing reactions thereof A 61 K 35 / 78 - Medicinal preparations containing substances of unspecified composition or producing their reactions, substances from plants A 61 K 31 / 00 - Medicinal preparations containing active organic ingredients Technical problem and solution to the technical problem The Mediterranean herbs myrtle (M. communis L.) and laurel (L. nobilis L.) have a long tradition of use in folk medicine for prevention and treatment of various gastrointestinal, urinary, dermatological and inflammatory diseases as well as injuries. These health The benefits stem from the presence of various bioactive molecules such as phenolic compounds, pigments, vitamins, sterols and volatile compounds accumulated in the form of essential oils in these plants. Due to all the above, these bioactive compounds are the subject of numerous scientific studies, with a particular focus on phenolic compounds due to their antioxidant effect. Myrtle and laurel leaf extracts stand out for their high content of phenolic compounds, with the leaf containing In myrtle, the most abundant flavan-3-ols and hydroxybenzoic acids are present, while in bay leaves, flavonols are the most abundant group. Since the phenolic compounds of these plants show structural diversity, this may affect their bioavailability, metabolism and bioactivity, with the gut microbiota playing a key role in modulating production, bioavailability, and thus the biological activities of phenolic metabolites. The technical problem solved by this invention is the process of obtaining myrtle (M. communis L.) and laurel (L. nobilis) extracts. L.) with high yield of phenolic compounds using cryogenic grinding as pretreatment, application of extraction assisted by microwaves (MAE) as an extraction technique and encapsulation of the produced extracts with application spray drying. State of the art In Croatia, no dietary supplement based on the symbiotic action of myrtle extract (M. communis L.) and laurel (L. nobilis L.) as a preparation intended to modulate intestinal microflora. The essence of the invention The process of obtaining the extract takes place in several steps; receiving and storing dried myrtle and laurel leaves, cryogenic milling, microwave extraction, concentration of plant extracts, mixing of extracts in the appropriate ratio, spray drying of plant extracts, filling the powder into capsules, packaging and storage capsules produced. Since bioactive molecules are often sensitive to elevated temperature, particle size reduction can be applied. grinding at low temperatures using nitrogen as a cryogen, i.e. cryogenic grinding. In this way it is possible preserve the biological value of plant material and achieve greater reduction and uniformity of particle size, which also increases the extraction yield. Extraction depends on many factors such as particle size, choice of extraction solvent, and method and conditions. extraction, Due to the well-known general principle of solubility, it is necessary to choose a polarity solvent for efficient extraction adapted to target bioactive molecules. Also, the application of microwave-assisted extraction (MAE) for the isolation of bioactive components from medicinal plants herbs have shown numerous advantages over classic extraction methods. The driving mechanism of such a procedure is microwave energy which leads to a rapid increase in the temperature of the solvent as well as the destruction of the structure of plant cells, which the result is a faster and easier release of bioactive molecules from the plant material into the extraction. The main characteristics of that The advantages of this method are significantly shorter extraction time, lower solvent consumption and higher yields of bioactive compounds. connections. Furthermore, the application of liquid extracts has certain limitations related to difficulties during incorporation and impact on the aroma and taste of food products and with low bioavailability of bioactive molecules. The above The disadvantages can be effectively overcome by using encapsulation methods, including spray drying. most widespread. During drying, the liquid extract is stabilized using high-molecular polysaccharides or food gums as carrier is dispersed in a stream of heated air and converted into a stable powder form. This protects the bioactive molecules from negative environmental impacts and consequent degradation, their incorporation into food matrices is facilitated, a bioavailability in the human body increased up to twofold. Description of the realization and application of the invention The developed extraction and encapsulation process of myrtle and laurel extracts enables optimal utilization of bioactive molecules-phenolic compounds and their stabilization and bioavailability. The process begins with the pretreatment of dry leaves myrtle and laurel, using cryogenic grinding in liquid nitrogen at -196 °C for 6 minutes. In this way, it achieves The micronization of plant material to a particle size of 40 to 50 μm allows for optimal contact with the extraction agents. solvent and increasing the extraction yield of phenolic compounds. Furthermore, a 30% aqueous solution of ethanol is used as the extraction solvent, which has been found by research to give maximum yields of phenolic compounds that were selected and monitored as target bioactive molecules in the produced extracts. The extraction of targeted bioactive molecules (phenolic compounds) from laurel and myrtle is carried out using microwave (MAE) for 10 minutes at 80 °C, at a microwave power of 400 W. The produced extracts are then evaporated on a vacuum concentrator (50 °C, 0.2 bar) where they are standardized to total phenol concentration of 25 g / L. In order to manifest the synergistic effect of these two plants, the standardized extracts are mixed in a volume ratio myrtle:laurel = 3:1 (v / v). Spray drying of the prepared mixture of myrtle and laurel extracts is carried out at a temperature of 180 °C, with the addition of combination of carrier β-cyclodextrin and maltodextin (1:1), in the ratio of sample and carrier 1:2 to the final proportion of dry matter of at least 95%. If the powder production is carried out on a laboratory spray dryer with a capacity of 1.0 L / h of evaporated water, aspirator capacity values ​​are adjusted to 80%, pump capacity 15% and nozzle cleaner to level 4. It is important to dry the extract mixture in such a way that the concentration of total phenols in the liquid keep the extract in the produced powder. The resulting powder is packaged in capsules in an amount of 1000 mg / capsule, which corresponds to a concentration of phenolic compounds of 55. mg / capsule, and the capsules are packaged in glass vials.

Claims

PATENT REQUESTS 1. Process for obtaining dry extract of phenolic compounds - bioactive molecules of medicinal herbs myrtle and laurel intended for modulation of intestinal microflora, characterized in that myrtle and laurel leaves are crushed using cryogenic grinding in liquid nitrogen at -196 °C for 6 minutes, then extraction of phenolic compounds is carried out compounds from laurel and myrtle in an extraction solvent, using microwaves for 10 minutes at 80 °C at microwave power of 400 W, after which the produced extracts are evaporated on a vacuum concentrator (50 °C, 0.2 bar) where they are standardized to a concentration of total phenols of 25 g / L, then mixed, dried and encapsulated in such a way that the resulting powder is packed into capsules in an amount of 1000 mg / capsule, which corresponds to the concentration of phenolic compounds of 55 mg / capsule.

2. Process for obtaining a dry extract of phenolic compounds from the medicinal herbs myrtle and laurel intended for modulation of intestinal microflora according to patent claim 1, characterized in that 30% aqueous solution is used as the extraction solvent ethanol solution.

3. Process for obtaining a dry extract of phenolic compounds from the medicinal herbs myrtle and laurel intended for modulation of intestinal microflora according to claim 1, characterized in that the process of mixing standardized extracts is carried out in a volume ratio of myrtle:laurel = 3:1 (v / v).

4. Process for obtaining a dry extract of phenolic compounds from the medicinal herbs myrtle and laurel intended for modulation of intestinal microflora according to claim 1, characterized in that the drying process is carried out by spray drying prepared mixtures of myrtle and laurel extracts at a temperature of 180 °C, with the addition of a combination of carriers β- cyclodextrin and maltodextrin (1:1), in a sample to carrier ratio of 1:2 to a final dry matter content of at least 95%. <addr> < / addr> Application / number: P20231354A Applicant: University of Zagreb, Faculty of Food Technology and Biotechnology (FFT), Pierottijeva ulica 6, 10000 Zagreb, Croatia Filing date: International application number: 25.10.2023. Priority date: Priority number: International Patent Classification (IPC): A23L 33 / 105, A23L 27 / 10, A61K 36 / 54, A61K 36 / 61, A61P 1 / 00, A61K 127 / 00 Searched areas (MKP): A23L, A61K, A61P Electronic database used in the search: SIPO database, Epodoc, Google DOCUMENTS CONSIDERED RELEVANT Relevant for Category* Citation of documents with indication of relevant parts, where appropriate patent application Y US20180264062A1 (MOLEAC PTE LTD [SG]); 20 September 2018 1-4 entire document ---- Y Tandara, Monika – “Retention of phenolic compounds in flower extract powders 1-4 blackberries during spray drying”, graduate thesis, University of Zagreb, Faculty of Food and Biotechnology, 2017. downloaded from https: / / urn.nsk.hr / urn:nbn:hr:159:299819 entire document ---- Y Jurić, M. – “Production of powdered plant extracts by spray drying”, 1-4 final thesis, University of Zagreb, Faculty of Food Technology and Biotechnology, 2017, retrieved from https: / / urn.nsk.hr / urn:nbn:hr:159:546886 entire document ---- A “Unexpected discovery by Croatian scientists: two plants from our climate 1-4 are extremely strong antioxidants and prebiotics"; 23.4.2023; taken from https: / / zivim.jutarnji.hr / zivim / ucim / neocekivano-otkrice-hrvatskih-znanstvenika- two-plants-from-our-climate-are-exceptionally-strong-antioxidants-and-prebiotics-15327150 entire document ---- A “Laurel, Dracena, Myrtle - Medicinal shrubs from the Adriatic coast”; 23.09.2014, taken 1-4 from https: / / gospodarski.hr / rubrike / ljekovito-bilje-rubrike / ljekoviti-grmovi-s- Adriatic-coast / The entire document, especially the section Bay leaf as a spice and the section Significance-Myrtle ---- <addr>* Categories of cited documents: X: particularly relevant to the novelty or inventive step of the invention if E: published on or after the filing date of the application (earlier the document itself is taken) Y: particularly relevant to the inventive step of the invention if T: published after the filing date or the date of the right combined with one or more documents of the same priority category (later document), and is cited in order to be understood A: defines the general state of the art, which is not specifically considered the principle or theory on which the invention is based relevant D: cited in the application A: refers to oral communication, use, exposition or some L: cited for other reasons another way …………………………………………. P: published before the filing date but after the granted &: belongs to the same patent family priority date Creation date:< / addr> October 18, 2024. Patent examiner: Blanka Grahovac Guberina, B.Eng. <addr>Form ST (September 2020)< / addr> 5 <addr>TD3451 <addr> < / addr> A Cvitković Daniela; Balbino Sandra – "Innovative and environmentally friendly techniques 1-4 extraction of bioactive molecules from myrtle (M. communis L.)" / / Zbornik sažetaka 1. scientific doctoral conference of the Faculty of Geotechnics '"Research in Environmental Engineering” / Loborec Jelena, Zavrtnik Saša; Varaždin, Croatia; Faculty of Geotechnical Engineering, University of Zagreb, 2021, pp. 14-15; retrieved from https: / / www.croris.hr / crosbi / publikacija / prilog-skup / 707233 abstract ---- <addr>* Categories of cited documents: X: particularly relevant to the novelty or inventive step of the invention if E: published on or after the filing date of the application (earlier the document itself is taken) Y: particularly relevant to the inventive step of the invention if T: published after the filing date or the date of the right combined with one or more documents of the same priority category (later document), and is cited in order to be understood A: defines the general state of the art, which is not specifically considered the principle or theory on which the invention is based relevant D: cited in the application A: refers to oral communication, use, exposition or some L: cited for other reasons another way …………………………………………. P: published before the filing date but after the granted &: belongs to the same patent family priority date Creation date:< / addr> October 18, 2024. Patent examiner: Blanka Grahovac Guberina, B.Eng. <addr> Form ST (September 2020)< / addr> 6 <addr> TD3451< / addr> < / addr>