Process for manufacturing a powdered food supplement based on liquid essential oils

Abstract

The present invention relates to a process for preparing a food supplement that is in the form of a powder and is based on at least one essential oil, as well as to said food supplement.

Description

Description Title: Manufacturing process for a powdered food supplement based on liquid essential oils Technical field

[0001] The present invention relates to methods of manufacturing food supplements presented in powder form based on liquid essential oils. Prior art

[0002] Products made from essential oils are perfect food supplements which, without being medicines, undoubtedly contribute to the well-being of living beings, human or otherwise. Technical problem

[0003] The problem that arises is that of their absorption by living beings. Indeed, the liquid form proves to be impractical, unpleasant due to the very strong tastes of essential oils, imprecise and potentially dangerous. Also, attempts have been made to produce these food supplements in solid form. Such a process is for example described in documents FR 2572935, FR 1402039, WO / 2006000652 and / or W02004 / 028550, possibly EP1938810, US2010 / 303990, DE102006056454 and FR2941846.

[0004] These documents do not describe processes that are easy to implement with means commonly available on the market and, above all, which make it possible to obtain satisfactory products for constituting powdered food supplements based on essential oils for the benefit of consumers.

[0005] All the results obtained to date are not really satisfactory, and the processes for producing these solids are relatively complex and therefore expensive. Summary of the invention

[0006] Also, the present invention aims to implement a method for manufacturing powdered food supplements based on essential oils which overcomes the drawbacks of the methods of the prior art.

[0007] More specifically, the present invention relates to a method for manufacturing a powdered food supplement based on at least one essential oil.

[0008] Other characteristics and advantages of the present invention will appear during the following description given with regard to an example of implementation of the method according to the invention for the manufacture of a powdered food supplement based on essential oils, this example of implementation being given below for illustrative purposes but in no way limiting. It is first of all specified that when, in the present description, an expression defines on its own, without any particular specific mention concerning it, a set of characteristics, these characteristics can be taken, for the definition of the object of the protection requested, when this is technically possible, either separately, or in total and / or partial combination. It is further specified that, in the present description, if the adverb "substantially" is associated with a qualifier of a means and / or of a datum, this qualifier must be understood in the strict or approximate sense or of the order of.

[0009] Essential oils, sometimes referred to as "plant essences," are well known. They are used in many areas of application, particularly for the well-being of living beings, both humans and animals. They consist of a concentrated, hydrophobic liquid made up of volatile aromatic compounds from a plant. These compounds are obtained exclusively by mechanical extraction, steam distillation, mechanical extraction, or dry distillation.

[0010] The present invention relates to a process for the manufacture of a powdered food supplement based on at least one essential oil. Thus, a first object of the invention is a process for preparing a food supplement in powder form comprising oyster shell powder and at least one essential oil, comprising the following steps: a) stirring an oyster shell powder; b) adding by spraying at least one essential oil to the oyster shell powder while stirring; c) stirring the mixture obtained at the end of step b); d) stirring the mixture obtained at the end of step c) at a pressure higher than atmospheric pressure; e) placing the mixture obtained at the end of step d) at atmospheric pressure, then adding an anti-caking agent and optionally a dry plant extract and stirring; f) leaving the product obtained at the end of step e) to stand to obtain the final product.

[0011] A second subject of the invention is a food supplement in powder form comprising oyster shell powder and at least one essential oil.

[0012] This food supplement in powder form is advantageously prepared according to the process of the invention. Statement of the invention

[0013] A first subject of the invention is a method for preparing a food supplement in powder form comprising oyster shell powder and at least one essential oil, comprising the following steps: a) stirring an oyster shell powder; b) adding by spraying at least one essential oil to the oyster shell powder while stirring; c) stirring the mixture obtained at the end of step b); d) stirring the mixture obtained at the end of step c) at a pressure higher than atmospheric pressure; e) placing the mixture obtained at the end of step d) at atmospheric pressure, then adding an anti-caking agent and optionally a dry plant extract and stirring; f) leaving the product obtained at the end of step e) to stand to obtain the final product.

[0014] This process first involves stirring a mineral powder from oyster shells. This step allows the powder to be dispersed and thus homogenizes the particles. It can be carried out at a speed of 2800 to 3200 rpm, preferably 3000 rpm, advantageously for a period of 45 to 75 minutes, preferably 60 minutes.

[0015] The entire process can be carried out in a mixer or a centrifuge. It is therefore possible to use a stand mixer, a paddle mixer or a spiral mixer. Said mixer or centrifuge are advantageously equipped with spray nozzles in order to add the essential oil or oils used in the composition of the prepared food supplement. Said mixer or centrifuge are also advantageously equipped with pressurization means. Furthermore, the entire process is advantageously carried out without the use of heating or a cooling system. However, since the process includes stirring steps, an increase in temperature inherent in the high-speed rotation may be observed.

[0016] Preferably, the powder used in step a) is a limestone powder very rich in calcium carbonate of marine origin consisting of crushed fragments of oyster shells.

[0017] This oyster shell powder preferably has a particle size distribution such that in a given sample 100% of the particles have a size less than 595 pm (measurements made according to the air jet sieving method). Said powder preferably has a density of 0.85 g / ml.

[0018] Preferably, the oyster shell will be a marine form, even more preferably fossilized marine. The fossilized form of this marine shell allows, during the ingestion of fossilized oyster shell powder, the complete solubilization in the digestive tract of the calcium carbonate that composes it due to the absence of a protein envelope (conchiolin) that protects it in a non-fossilized form. The calcium carbonate is thus more efficiently absorbed in the small intestine.

[0019] The interest of this form of oyster shell is also the fact that it is rich in minerals and especially in trace elements. It is particularly rich in calcium with a content of at least 38% by mass compared to the mass of the oyster shell. It also contains many trace elements such as iodine, sulfur, iron, manganese, zinc, selenium, boron, copper, cobalt.

[0020] It can therefore be used in the manufacture of an ideal food supplement containing trace elements essential to the good health of the human body. Its high calcium carbonate content allows in particular a supply of alkaline elements in the form of bicarbonate ions allowing the optimal regulation of the acid-base balance of the blood serum. A lasting excess of tissue acidity forces the body to draw on its alkaline reserves, particularly bone reserves. When it persists, such a mechanism therefore promotes demineralization, even osteoporosis and the loss of essential minerals (Calcium, Magnesium, Potassium). This correction of metabolic acidosis allows in particular to maintain good bone capital.

[0021] It is this solution combining essential oils and calcium carbonate of marine origin that allows the optimal expression of the properties of the different essential oils on organisms in a chronic state of metabolic acidosis. This intake of calcium carbonate in the form of oyster shell can therefore, on the one hand, be used regularly as a food supplement to recover from the various deficiencies that can appear due to poor diet or lifestyle, and on the other hand, be used to act on several problems at the level of the human body.

[0022] The second step of the process according to the invention (step b)) consists of adding at least one essential oil to the oyster shell powder while stirring by spraying.

[0023] This step can advantageously be carried out at a speed of 4300 to 4700 rpm, preferably 4500 rpm. It makes it possible to obtain a mixture of oyster shell powder / essential oil in a state which can be described as semi-pasty.

[0024] For the purposes of the present invention, the terms "essential oil" must be understood in their commonly accepted sense. Thus, it is well known that an essential oil is a "volatile odorous substance produced by certain plants and which can be extracted in the form of a liquid obtained by steam distillation of aromatic plants (leaves, flowers, bark, seeds, stems, etc.) the most widely used extraction method." (Definition of the General Directorate for Competition, Consumer Affairs and Fraud Control, https: / / www.economie.gouv.fr / dgccrf / Publications / Vie-pratique / Fiches- pratiques / Huiles-essentielles).Furthermore, the authorization of an essential oil for food is defined in a regulatory manner by a French decree (article 7 of decree n°2006-352) and a European regulation (article 14 of regulation (EC) n°178 / 2002), this information being made available to the public by the DGCCRF, Directorate General for Competition, Consumer Affairs and Fraud Control, (https: / / www.economie.gouv.fr / dgccrf / complements-alimentaires-huiles-essentiels).

[0025] The essential oil used is chosen very advantageously from the following essential oils: true lavender, verbenone rosemary, thyme, green anise, tea tree, lemon, cajuput, lemon eucalyptus, Scots pine, bay leaf, oregano, cinnamon, lemongrass, eucalyptus citriodora, Chinese star anise, fennel, green anise, goosefoot, Eucalyptus Globulus, sage, thuja, camphor, thyme, savory, clove, oregano, juniper, lemon, coriander, rosewood, mint, cruciferous and lily or any other essential oil authorized in food, or a mixture of at least two of these essential oils.

[0026] The oyster shell powder / essential oil mixture obtained after step b) is then kept stirring (step c)) in order to obtain good dispersion of the essential oil(s) in the oyster shell powder and thus have the most homogeneous mixture possible. This step is advantageously carried out at a speed of 4300 to 4700 rpm, preferably 4500 rpm, for a period of time ranging from 0 to 75 minutes, preferably from 0 to 60 minutes, for example 0 or 60 minutes. It makes it possible to obtain a mixture of oyster shell powder / essential oil in a state that is still pasty, but which can however be described as a little thicker.

[0027] The method according to the invention further comprises a step d) of stirring the mixture obtained at the end of step c) at a pressure higher than atmospheric pressure. This step is advantageously carried out at a speed of 2800 to 3200 rpm, preferably 3000 rpm, under a pressure of 2.8 to 3.2 bars, preferably 3 bars, for a period of time ranging from 3 to 5 hours, preferably 4 hours. This step is advantageously carried out under a neutral gas atmosphere, preferably air, but also possibly under nitrogen or carbon dioxide. The pressure higher than atmospheric pressure applied during this step makes it possible to obtain a better mixture of the components used. This step d) makes it possible to obtain an oyster shell powder / essential oil mixture in a state which is in the form of a "wet powder".

[0028] For the purposes of the present invention, atmospheric pressure means ambient pressure without the application of additional pressure or vacuum.

[0029] For the purposes of the present invention, the term “neutral gas” means a gas which does not react with the components of the mixture.

[0030] Step d) of the process according to the invention is followed by a step e), during which the oyster shell powder / essential oil mixture obtained at the end of step d) is brought back to atmospheric pressure. It is then still in the form of a "wet powder".

[0031] Then, still in step e), an anti-caking agent and optionally a dry plant extract are added to the mixture obtained after step d), and the mixture obtained is stirred. Stirring is advantageously carried out at a speed of 4800 to 5200 rpm, preferably 5000 rpm, for a period of 12 to 18 minutes, preferably 15 minutes.

[0032] The anti-caking agent added at this stage can advantageously be magnesium stearate, silicon dioxide in the form of colloidal silica, any other anti-caking agent authorized for human consumption, or a mixture of these compounds.

[0033] Preferably, the dry plant extract is chosen from dry extracts of terrestrial or maritime plants. A single dry plant extract or a mixture of at least two different extracts may be used. Examples of terrestrial plants include lemon balm, hop cone, green oregano, cranberry, thyme, lavender or any other dry extract of medicinal plant. It may also be a dry mushroom extract. Examples of dry extracts of maritime plants include dry extracts of algae, such as Ulva sp. (sea lettuce).

[0034] For the purposes of the present invention, the terms "medicinal plant" must be understood in their commonly accepted meaning. Thus, it is well known that "medicinal plants are plant drugs within the meaning of the European Pharmacopoeia (1433) at least one part of which has medicinal properties" (definition of the ANSM, French National Agency for the Safety of Medicines and Health Products, (https: / / ansm.sante.fr / uploads / 2020Z10 / 22 / plantes-medicinales.pdf). Furthermore, the ANSM makes available to the public on its website the list of medicinal plants used traditionally (https: / / ansm.sante.fr / pharmacopee / liste-des-plantes-medicinales-utilisees-traditionnellement).

[0035] The mixture obtained at the end of step e) of the process is then left to stand to obtain the final product which constitutes the desired food supplement in the form of a powder to which a mixture of essential oil(s) is fixed. This step of resting the product is advantageously carried out for a period ranging from 20 to 28 hours, preferably 24 hours, before packaging the final product.

[0036] Advantageously, to obtain a food supplement having optimal qualities, the proportions by weight of the components, respectively the oyster shell powder, the essential oil, the anti-caking agent and optionally the dry plant extract in the final product obtained according to the process of the invention are as follows: - from 10 to 75%, preferably from 15 to 70% of oyster shell powder; - from 5 to 35%, preferably from 10 to 30% of essential oil; - from 0.5 to 3% anti-caking agent; - from 0 to 70%, preferably from 0 to 65% of dry plant extract.

[0037] It is also preferable that the dry plant extract be an extract of the order of 5 / 1 (prepared by dehydrating a plant to divide its weight by 5), that is to say that one unit of weight of dry extract is equivalent on average to five units of plant powder before drying.

[0038] To ensure good conservation of the final powder mixture thus obtained and to facilitate its distribution, it is then possible, and advantageous, to package it in capsules or gelcaps, preferably in gelcaps.

[0039] The present invention also relates to a food supplement in powder form comprising oyster shell powder and at least one essential oil.

[0040] The food supplement in powder form according to the invention preferably comprises oyster shell powder which is a powder of marine oyster shell, preferably fossilized marine oyster.

[0041] The essential oils that can be used for the food supplement according to the invention are those described above in relation to the preparation process according to the invention. The food supplement in powder form according to the invention advantageously comprises, and in one embodiment consists of: - from 10 to 75%, preferably from 15 to 70% of oyster shell powder; - from 5 to 35%, preferably from 10 to 30% of essential oil; - from 0.5 to 3% anti-caking agent; - from 0 to 70%, preferably from 0 to 65% of dry plant extract., The percentages are expressed by weight relative to the total weight of the food supplement.

[0042] The food supplement in powder form according to the invention can be obtained by the process described above. Examples

[0043] Example 1: Implementation of the method according to the invention 21,050 kg of fossilized oyster shell powder was introduced into a mixer and stirred at a speed of 3000 rpm for 1 hour. 1.245 kg of thyme essential oil, 1 kg of rosemary essential oil, 0.934 kg of eucalyptus essential oil, 0.934 kg of tea tree essential oil, 0.623 kg of cinnamon essential oil, 0.623 kg of Scots pine needle essential oil, were then added to the fossilized oyster shell powder under stirring gradually and successively by spraying, then the mixture obtained was stirred at a speed of 4500 rpm for 4 hours at a pressure of 3 bars To the resulting mixture was then added a mixture of 7,470 kg of dry extract of holy basil, and 1,250 kg of anti-caking agent in the form of silicon dioxide and magnesium stearate, with a mixing speed of 5000 rpm for approximately 15 minutes at atmospheric pressure.

[0044] Approximately 35 kg of finished product powder is then collected and stored in an airtight storage container for 24 hours before the capsule filling operation.

[0045] Example 2: Comparative study of the calcium carbonate content of lithothamnium and fossilized oyster shell

[0046] [Table 1]

[0047] Conclusions: The results confirm the low calcium content of the Lithothamnium (34.89%) versus 41.6% for fossilized oyster shell

[0048] The results show the very low sodium content of fossilized oyster shell compared to lithothamnion 22mg / 100g versus 604mg / 100g for Lithothamnion.

[0049] The results show the very low content of major heavy metals in fossilized oyster shell compared to lithothamnium.

[0050] As for the other minerals analyzed, we can see interesting and balanced contributions of Strontium, Barium and Manganese from the fossilized oyster shell, trace elements naturally little present in the forms of contribution of terrestrial origin.

[0051] General conclusions: These analyses confirm the importance of the diagenesis undergone by oyster shells during fossilization, which leads to the almost total disappearance of the organic matter present in the fresh shell in the form of conchiolin, an organic matter which constitutes the crystallization matrix of the mineral fractions of oysters (calcite and aragonite).

[0052] Under these conditions, calcium carbonate, which represents more than 97% of the fossilized oyster shell, is much more absorbable in the small intestine and can therefore perfectly play its role in maintaining or correcting the body's acid-base balance.

[0053] The other results confirm on the one hand the very low heavy metal content of the fossilized oyster shell and the interest of its contribution in essential marine trace elements.

[0054] Example 3: Comparative study of the solubility of calcium carbonate from lithothamnium and fossilized oyster shell

[0055] Objective: Comparison of the solubilization capacities of calcium carbonate from two raw materials a priori rich in CaCO3, namely lithothamnium and fossilized oyster shell. General protocol: Dissolving the two products in powder form in beakers in demineralized water at controlled pH (target pH 6). Continuous controlled stirring of the solution in the beakers for 1 hour with pH rectification every 5 minutes. After one hour, collect the solutions and pass them through a filter. Weighing of residues after drying.

[0056] The weight of residue corresponds to the fraction not dissolved in the solution. Steps for carrying out the test:

[0057] 100ml of water was placed in a beaker containing a magnet. The whole thing was placed on a stirrer that was put into operation from the start of the test.

[0058] The pH of the water was adjusted to approximately 5.5 using hydrochloric acid. To avoid lowering the pH too quickly, the hydrochloric acid was diluted with demineralized water.

[0059] 2.5 g of each powder from the 2 products were added to the 2 beakers. (The 2.5 g corresponds to approximately 2 times the daily dosage recommendations for these products).

[0060] The pH of the product was measured every 5 minutes and adjusted to around 6 by adding hydrochloric acid.

[0061] After one hour, the stirring was stopped and the contents of the beakers were transferred into filter paper (each filter having been previously weighed).

[0062] The filter was then left to dry in an oven.

[0063] The filter containing the dry product residue was weighed and then the weight of the filter was subtracted from this weight.

[0064] The results of the test are presented in the table below.

[0065] [Table 2] Conclusions:

[0066] This study shows that under test conditions that replicate the environmental parameters of the first part of the small intestine, fossilized oyster shell is 100% soluble. Under the same conditions, lithothamnium powder is soluble at 56.50%. This confirms the importance of the diagenesis undergone by oyster shells during fossilization, which leads to the almost total disappearance of the organic matter present in the fresh shell in the form of conchiolin, an organic matter which constitutes the matrix of the mineral fractions.

[0067] Under these conditions, calcium carbonate, which represents more than 97% of the fossilized oyster shell, is 100% absorbable in the small intestine and can therefore perfectly play its role in maintaining or correcting the acid-base balance of the body.

Claims

Claims

1. A method for preparing a food supplement in powder form comprising oyster shell powder and at least one essential oil, comprising the following steps: a) stirring an oyster shell powder; b) adding by spraying at least one essential oil to the oyster shell powder while stirring; c) stirring the mixture obtained at the end of step b); d) stirring the mixture obtained at the end of step c) at a pressure higher than atmospheric pressure; e) placing the mixture obtained at the end of step d) at atmospheric pressure, then adding an anti-caking agent and optionally a dry plant extract and stirring; f) leaving the product obtained at the end of step e) to stand to obtain the final product.

2. The method of claim 1, wherein the oyster shell powder is marine fossilized oyster shell powder.

3. Method according to one of claims 1 or 2, for which the essential oil is chosen from the essential oils of true lavender, verbenone rosemary, thyme, green anise, tea tree, lemon, cajuput, lemon eucalyptus, Scots pine, bay leaf, oregano, cinnamon, lemongrass, eucalyptus citriodora, Chinese star anise, fennel, green anise, goosefoot, Eucalyptus Globulus, sage, thuja, camphor, thyme, savory, clove, oregano, juniper, lemon, coriander, rosewood, mint, cruciferous and lily plants or any other essential oil authorized for food, or a mixture of at least two of these essential oils.

4. Method according to one of claims 1 to 3, for which the dry plant extract is chosen from dry extracts of lemon balm, hop cone, green oregano, cranberry, or any other dry extract of medicinal plant, or a mixture of at least two of these dry extracts.

5. Method according to one of claims 1 to 4, for which the proportions by weight of the components of the final product relative to the weight of the final product are as follows: - from 10 to 75%, preferably from 15 to 70% of oyster shell powder; - from 5 to 35%, preferably from 10 to 30% of essential oil; - from 0.5 to 3% anti-caking agent; - from 0 to 70%, preferably from 0 to 65% of dry plant extract.

6. Method according to one of claims 1 to 5, for which step a) is carried out at a speed of 2800 to 3200 revolutions / minute, preferably 3000 revolutions / minute, for a duration ranging from 45 to 75 minutes, preferably 60 minutes.

7. Method according to one of claims 1 to 6, for which step b) is carried out at a speed of 4300 to 4700 revolutions / minute, preferably 4500 revolutions / minute.

8. Method according to one of claims 1 to 7, for which step c) is carried out at a speed of 4300 to 4700 revolutions / minute, preferably 4500 revolutions / minute, for a duration ranging from 0 to 75 minutes, preferably from 0 to 60 minutes.

9. Method according to one of claims 1 to 8, for which step d) is carried out at a speed of 2800 to 3200 revolutions / minute, preferably 3000 revolutions / minute, under a pressure of 2.8 to 3.2 bars, preferably 3 bars, for a duration ranging from 3 to 5 hours, preferably 4 hours.

10. Method according to one of claims 1 to 9, for which step e) is carried out at a speed of 4800 to 5200 revolutions / minute, preferably 5000 revolutions / minute, for a duration ranging from 12 to 18 minutes, preferably 15 minutes.

11. Method according to one of claims 1 to 10, for which step f) is carried out for a period ranging from 20 to 28 hours, preferably 24 hours.

12. Method according to one of claims 1 to 11, for which the final product obtained after step f) is packaged in the form of gelatin capsules.

13. Food supplement in powder form comprising oyster shell powder and at least one essential oil.

14. A powdered dietary supplement according to claim 13, wherein the oyster shell powder is a marine fossilized oyster shell powder.

15. Food supplement in powder form obtained by the process according to one of claims 1 to 12.

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