Manufacturing process for a powdered food supplement based on liquid essential oils.

Abstract

The present invention relates to a method for preparing a food supplement in powder form based on at least one essential oil, as well as said food supplement.

Description

Title of the invention: Process for manufacturing a powdered food supplement based on liquid essential oils. Technical field

[0001] The present invention relates to methods for 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 similar. Technical problem

[0003] The problem that arises is that of their absorption by living organisms. Indeed, the liquid form proves impractical, unpleasant due to the very strong tastes of essential oils, imprecise, and potentially dangerous. Therefore, attempts have been made to produce these food supplements in solid form. Such a process is described, for example, in documents FR 2572935, FR 1402039, WO / 2006000652 and / or WO2004 / 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, that allow for obtaining 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 truly 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 process for manufacturing powdered food supplements based on essential oils which overcomes the disadvantages of prior art processes.

[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 features and advantages of the present invention will become apparent from the following description given in relation to an example of an implementation of the process according to the invention for the manufacture of a powdered food supplement based on essential oils, this example of implementation being given below by way of illustration but in no way limiting. It is first specified that when, in this description, an expression defines on its own, without further specification specific to it, a set of characteristics; these characteristics may be taken, for the definition of the subject matter of the protection sought, when technically possible, either separately or in total and / or partial combination. It is further specified that, in this description, if the adverb "significantly" is associated with a qualifier of a means and / or data, this qualifier must be understood in its strict or approximate sense, or in the order of.

[0009] Essential oils, sometimes referred to as "plant essences," are well known. They are used in numerous fields 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 derived from a plant. These compounds are obtained exclusively by mechanical extraction, steam distillation, or dry distillation.

[0010] The present invention relates to a process for manufacturing a powdered food supplement based on at least one essential oil.

[0011] 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:

[0012] a) to stir an oyster shell powder;

[0013] b) add by spraying at least one essential oil to the shell powder oyster under agitation;

[0014] c) stir the mixture obtained at the end of step b);

[0015] d) agitate the mixture obtained at the end of step c) at a pressure greater than the atmospheric pressure;

[0016] e) place the mixture obtained at the end of step d) at atmospheric pressure, then add an anti-caking agent and optionally a dry vegetable extract and shake;

[0017] f) let the product obtained at the end of step e) rest to obtain the final product.

[0018] A second object of the invention is a food supplement in powder form including oyster shell powder and at least one essential oil.

[0019] This food supplement in powder form is advantageously prepared according to the process of the invention. Description of the invention

[0020] 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:

[0021] a) to stir an oyster shell powder;

[0022] b) add by spraying at least one essential oil to the shell powder oyster under agitation;

[0023] c) stir the mixture obtained at the end of step b);

[0024] d) agitate the mixture obtained at the end of step c) at a pressure greater than the atmospheric pressure;

[0025] e) place the mixture obtained at the end of step d) at atmospheric pressure, then add an anti-caking agent and optionally a dry vegetable extract and shake;

[0026] f) let the product obtained at the end of step e) rest to obtain the final product.

[0027] This process first consists of agitating a mineral powder obtained from Oyster shell. This step disperses the powder, thus homogenizing the particles. It can be carried out at a speed of 2800 to 3200 rpm, preferably 3000 rpm, advantageously for a duration of 45 to 75 minutes, preferably 60 minutes.

[0028] The entire process can be carried out in a mixer or centrifuge. It is therefore possible to use a base mixer, a paddle mixer, or a spiral mixer. The mixer or centrifuge is advantageously equipped with spray nozzles for adding the oil or essential oils used in the preparation of the food supplement. The mixer or centrifuge is also advantageously equipped with pressurization means. Furthermore, the entire process is advantageously carried out without the need for heating or cooling. However, since the process includes stirring steps, a temperature increase inherent to high-speed rotation may occur.

[0029] Preferably, the powder used in step a) is a very rich calcium carbonate limestone powder of marine origin made up of crushed fragments of oyster shells.

[0030] 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 µm (measurements taken using the airjet sieving method). The powder preferably has a density of 0.85 g / ml.

[0031] Preferably, the oyster shell will be a marine form, and even more preferably a fossilized marine form. The fossilized form of this marine shell allows, upon ingestion of fossilized oyster shell powder, the complete solubilization in the digestive tract of the calcium carbonate it contains, due to the absence of the protein coat (conchiolin) that protects it in a non-fossilized form. The calcium carbonate is thus more efficiently absorbed in the small intestine.

[0032] The advantage of this type of oyster shell is also that it is rich in minerals and especially trace elements. It is particularly rich in calcium with a minimum content of 38% by mass relative to the mass of the oyster shell. It also contains numerous trace elements such as iodine, sulfur, iron, manganese, zinc, selenium, boron, copper, and cobalt.

[0033] It can therefore be used in the manufacture of an ideal food supplement containing trace elements essential for good human health. Its high calcium carbonate content, in particular, provides alkaline elements in the form of bicarbonate ions, allowing for optimal regulation of the acid-base balance of blood serum. A prolonged excess of tissue acidity forces the body to draw on its alkaline reserves, especially those in bone. When this mechanism persists, it promotes demineralization, even osteoporosis, and the loss of essential minerals (calcium, magnesium, potassium). This correction of metabolic acidosis helps, in particular, to maintain good bone health.

[0034] It is this solution, combining essential oils and marine-derived calcium carbonate, that allows for the optimal expression of the properties of the various essential oils on organisms in a chronic state of metabolic acidosis. This supply of calcium carbonate in the form of oyster shell can therefore, on the one hand, be used regularly as a food supplement to address various deficiencies that may arise due to poor diet or lifestyle, and on the other hand, be used to address several issues affecting the human body.

[0035] The second step of the process according to the invention (step b)) consists of adding at least one essential oil by spraying to the oyster shell powder while stirring.

[0036] 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 powdered oyster shell / essential oil mixture in a semi-pasty state.

[0037] The essential oil used is most advantageously chosen from among the following essential oils: true lavender, rosemary verbenone, thyme, green anise, tea tree, lemon, cajeput, lemon eucalyptus, Scots pine, bay, oregano, cinnamon, lemongrass, eucalyptus citriodora, Chinese star anise, fennel, green anise, goosefoot, Eucalyptus globulus, sage, thuja, camphor tree, thyme, savory, clove, oregano, juniper, lemon, coriander, rosewood, mint, cruciferous and liliaceae or any other essential oil authorized in food, or a mixture of at least two of these essential oils.

[0038] The oyster shell powder / essential oil mixture obtained after step b) is then kept under agitation (step c)) in order to obtain good dispersion of the essential oil or essential oils in the oyster shell powder and thus The goal is to achieve the most homogeneous mixture possible. This step is advantageously carried out at a speed of 4300 to 4700 rpm, preferably 4500 rpm, for a duration of 0 to 75 minutes, preferably 0 to 60 minutes, for example, 0 to 60 minutes. This process yields a powdered oyster shell / essential oil mixture that is still pasty, but can nevertheless be described as slightly thicker.

[0039] The process 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 bar, preferably 3 bar, for a period of 3 to 5 hours, preferably 4 hours. This step is advantageously carried out under an atmosphere of neutral gas, preferably air, but also possibly under nitrogen or carbon dioxide. The pressure higher than atmospheric pressure applied during this step allows for better mixing of the components used. This step d) makes it possible to obtain a mixture of oyster shell powder / essential oil in a state that is in the form of a "wet powder".

[0040] For the purposes of the present invention, atmospheric pressure means ambient pressure without the application of additional pressure or a vacuum.

[0041] For the purposes of the present invention, a neutral gas is understood to be a gas which does not react with the components of the mixture.

[0042] 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".

[0043] 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 resulting mixture 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.

[0044] The anti-caking agent added at this stage may advantageously be magnesium stearate, silicon dioxide in the form of colloidal silica, any other anti-caking agent authorized in human food, or a mixture of these compounds.

[0045] Preferably, the dry plant extract is chosen from dry extracts of terrestrial or marine 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, oregano, cranberry, thyme, lavender, or any other medicinal plant extract. It may also be a dry mushroom extract. As Examples of dry extracts of marine plants include dry extracts of algae, such as Ulva sp. (sea lettuce).

[0046] The mixture obtained at the end of step e) of the process is then left to rest, 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 / are fixed. This resting step is advantageously carried out for a period of 20 to 28 hours, preferably 24 hours, before packaging the final product.

[0047] Advantageously, to obtain a food supplement with optimal qualities, the proportions by weight of the components, respectively oyster shell powder, essential oil, anti-caking agent and optionally dry plant extract in the final product obtained according to the process of the invention are as follows: - 10 to 75%, preferably 15 to 70% oyster shell powder; - 5 to 35%, preferably 10 to 30% essential oil; - 0.5 to 3% anti-caking agent; - from 0 to 70%, preferably from 0 to 65% dry vegetable extract.

[0048] 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.

[0049] To ensure good preservation of the final powder mixture thus obtained and to facilitate its distribution, it is then possible, and advantageous, to package it in capsules or softgels, preferably in softgels.

[0050] The present invention also relates to a food supplement in powder form comprising oyster shell powder and at least one essential oil.

[0051] The food supplement in powder form according to the invention preferably comprises oyster shell powder which is a powder of marine oyster shell, preferably of fossilized marine oyster.

[0052] 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.

[0053] The powdered food supplement according to the invention advantageously comprises, and in one embodiment consists of:

[0054] - from 10 to 75%, preferably from 15 to 70% oyster shell powder;

[0055] - from 5 to 35%, preferably from 10 to 30% essential oil;

[0056] - from 0.5 to 3% anti-caking agent;

[0057] - from 0 to 70%, preferably from 0 to 65% dry vegetable extract.

[0058] The percentages are expressed as a percentage of the total weight of the food supplement.

[0059] The food supplement in powder form according to the invention can be obtained by the process described above. Examples

[0060] Example 1: Implementation of the process according to the invention

[0061] 21.050 kg of fossilized oyster shell powder were introduced into a blend and stirred at a speed of 3000 revolutions per minute for one hour.

[0062] 1.245 kg of thyme essential oil, 1 kg of rosemary essential oil, 0.934 kg 0.934 kg of eucalyptus essential oil, 0.623 kg of tea tree essential oil, 0.623 kg of cinnamon essential oil, and 0.623 kg of Scots pine needle essential oil were then added to the fossilized oyster shell powder while stirring, gradually and successively by spraying. The resulting mixture was then stirred at a speed of 4500 rpm for 4 hours at a pressure of 3 bars.

[0063] To the mixture obtained were 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 revolutions / minute for about 15 minutes at atmospheric pressure.

[0064] Approximately 35kg of finished product powder are then recovered and stored in an airtight storage container for 24 hours before the encapsulation operation.

[0065] Example 2: Comparative study of the calcium carbonate content of lithothamnium and fossilized oyster shell

[0066] [Tables 1] Elements analyzed: Content in the fossilized oyster shell: Content in the Li-thothamnium: Arsenic: Method: AS UL 00.00.135, ICP-MS 0.15 mg / kg 3.9 mg / kg; Lead: Method: AS UL 00.00.135, ICP-MS 0.083 mg / kg 0.7 mg / kg; Cadmium: Method: AS UL 00.00.135, ICP-MS 0.37 mg / kg 0.46 mg / kg; Mercury: Method: AS UL 00.00.135, ICP-MS 0.0020 mg / kg 0.0020 mg / kg; Calcium: Method: AS UL 00.00-144, ICP-OES 41605 mg / 100 g 34890 mg / 100 g; Sodium: Method: AS UL 00.00-144, ICP-OES 0.022 g / 100 g 0.604 g / 100 g Aluminum Method: AS EU 00.00-144, ICP-OES 68.8 mg / kg 3384 mg / kg Sulfur Method: PV-SA-092, HPLC-UV 0.6 mg / kg 9825 mg / kg Iron Method: AS EU 00.00-144, ICP-OES 72 mg / kg 4090 mg / kg Strontium Method: PV-SA-337, ICP-MS 208.1 mg / kg 1607.5 mg / kg Barium Method: AS EU 45.0 mg / kg 9.46 mg / kg 00.00-144, ICP-OES Manganese Method: AS UL 00.00-144, ICP-OES 15.5 mg / kg 93.5 mg / kg

[0067] Conclusions: The results confirm the low calcium content of Lithothamnium (34.89%) compared to 41.6% for the fossilized oyster shell

[0068] The results show the very low sodium content of the fossilized oyster shell compared to the lithothamnium 22mg / 100g versus 604mg / 100g for the Lithothamnium.

[0069] The results show the very low content of major heavy metals in the fossilized oyster shell compared to the lithothamnium.

[0070] 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 present in small amounts in forms of terrestrial origin.

[0071] 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, organic matter which constitutes the crystallization matrix of the mineral fractions of oysters (calcite and aragonite).

[0072] 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 acid-base balance of the body.

[0073] The other results confirm on the one hand the very low content of heavy metals in the fossilized oyster shell and the interest of its contribution of essential marine trace elements.

[0074] Example 3: Comparative study of the solubility of calcium carbonate from lithothamnium and fossilized oyster shell

[0075] Objective: Comparison of the calcium carbonate solubilization capacities of 2 raw materials a priori rich in CaCO3, namely lithothamnium, and fossilized oyster shell. General protocol:

[0076] Dissolving the two products in powder form in demineralized water at a controlled pH (target pH 6) in beakers. Continuous controlled stirring of the solution in the beakers for 1 hour with pH adjustment every 5 minutes.

[0077] After one hour, recovery of the solutions and passing through a filter.

[0078] Weighing of residues after drying.

[0079] The weight of residues corresponds to the fraction not solubilized in the solution. Steps in conducting the test:

[0080] 100 ml of water are placed in a beaker containing a magnet. The whole thing has been placed on an agitator put into operation from the start of the test.

[0081] 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.

[0082] 2.5 g of each powder of the 2 products were added to the 2 beakers. (The 2.5 g corresponding to approximately 2 times the recommended daily dosage of these products).

[0083] The pH of the product was measured every 5 minutes and adjusted to around 6 by adding hydrochloric acid.

[0084] After one hour the stirring was stopped and then the contents of the beakers were transferred into filter paper (each filter having been previously weighed).

[0085] The filter was then placed in an oven to dry.

[0086] The filter containing the dry product residue was weighed and then the weight of the filter was subtracted from that weight.

[0087] The results of the test are presented in the table below.

[0088] [Tables2] Filter weight in g Total dry weight in g Weight of insoluble residue in g % of solubilized product LITHOTHAMNE 1.665 2.751 1.086 56.50% C. FOSSILIZED OYSTER 1.664 1.664 0.000 100% Conclusions:

[0089] This study shows that under the test conditions which reproduce the environmental parameters of the first part of the small intestine the fossilized oyster shell is 100% soluble.

[0090] Under the same conditions, the lithothamnium powder is 56.50% soluble.

[0091] This confirms the significant interest of the diagenesis undergone by oyster shells during of fossilization which leads to the almost total disappearance of the organic matter present in the fresh shell in the form of conchiolin, organic matter which constitutes the matrix of the mineral fractions.

[0092] 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

[0093] the organism.

Claims

Demands

1. 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 oyster shell powder; b) spraying at least one essential oil onto 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 above 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) allowing the product obtained at the end of step e) to settle to obtain the final product.

2. A method according to claim 1, wherein the oyster shell powder is a marine fossilized oyster shell powder.

3. A process according to any one of claims 1 or 2, wherein the essential oil is selected from the essential oils of true lavender, rosemary verbenone, thyme, green anise, tea tree, lemon, cajeput, lemon eucalyptus, Scots pine, bay, oregano, cinnamon, lemongrass, eucalyptus citriodora, Chinese star anise, fennel, green anise, goosefoot, Eucalyptus globulus, sage, thuja, camphor tree, thyme, savory, clove, oregano, juniper, lemon, coriander, rosewood, mint, cruciferous and liliaceae or any other essential oil authorized for use in food, or a mixture of at least two of these essential oils.

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

5. A process according to any one of claims 1 to 4, wherein 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% oyster shell powder; - from 5 to 35%, preferably from 10 to 30% essential oil; - from 0.5 to 3% anti-caking agent; - from 0 to 70%, preferably from 0 to 65% dry vegetable extract.

6. A method according to any one of claims 1 to 5, wherein step a) is carried out at a speed of 2800 to 3200 rpm, preferably 3000 rpm, for a period of 45 to 75 minutes, preferably 60 minutes.

7. A method according to any one of claims 1 to 6, wherein step b) is carried out at a speed of 4300 to 4700 rpm, preferably 4500 rpm.

8. A method according to any one of claims 1 to 7, wherein step c) is carried out at a speed of 4300 to 4700 rpm, preferably 4500 rpm, for a period of 0 to 75 minutes, preferably 0 to 60 minutes.

9. A method according to any one of claims 1 to 8, wherein step d) is carried out at a speed of 2800 to 3200 rpm, preferably 3000 rpm, under a pressure of 2.8 to 3.2 bar, preferably 3 bar, for a period of 3 to 5 hours, preferably 4 hours.

10. A method according to any one of claims 1 to 9, wherein step e) is carried out at a speed of 4800 to 5200 rpm, preferably 5000 rpm, for a period of 12 to 18 minutes, preferably 15 minutes.

11. A method according to any one of claims 1 to 10, wherein step f) is carried out for a period of 20 to 28 hours, preferably 24 hours.

12. A method according to any one of claims 1 to 11, wherein the final product obtained after step f) is packaged in the form of capsules or caplets.

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

14. A food supplement in powder form according to claim 13, wherein the oyster shell powder is a marine fossilized oyster shell powder.

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