Method for obtaining extract from red hot pepper

Abstract

FIELD: oil and fat industry.SUBSTANCE: method is proposed for obtaining an extract from red hot pepper, characterized in that the extraction is carried out in two stages, wherein in the first stage fresh or dried whole red pepper pods are extracted with a 30% aqueous solution of ethyl alcohol, and in the second stage the pepper pods are crushed and again extracted with the extract obtained in the first stage, the extract obtained after two stages is drained, wherein when using fresh pepper the amount of pepper is 8400 g, and the amount of 30% aqueous solution of ethyl alcohol is 9600 g, and when using dried pepper the amount of pepper is 1000 g, and the amount of 30% aqueous solution of ethyl alcohol is 11500 g.EFFECT: obtaining an extract from red pepper with a high content of capsaicinoids.1 cl, 1 tbl, 3 ex

Description

[0001] The invention relates to the technology of extracting plant raw materials containing capsaicin and can be used in the food, medical and perfumery and cosmetic industries.

[0002] It is known that capsaicin (C18H27NO3), which belongs to the pharmacological group of "Natural irritants", has an irritating effect on the upper respiratory tract, skin and mucous membranes that is hazardous to human health when administered above certain doses. Moreover, the acute toxicity of capsaicin upon oral administration is 47.2 mg / kg of mouse weight, and the acute toxicity upon contact with skin is more than 512 mg / kg of mouse weight [Rudometova N.V., Kim I.S. Study of capsaicin extraction from the fruits of hot peppers of the genus Capsicum / / Scientific journal of NRU ITMO. Series "Processes and equipment for food production". - 2019. - No. 1. - P. 62-73]. Capsaicin's irritant and analgesic effects are due to its action on vanilloid receptors, of which it is an agonist. The average person's tolerance to capsaicin is 0.004 mg / dm³ in a food drink after two minutes of exposure [Asaturov Yu.V., Semkina O.A., Dul V.N.Identification and extraction of the main biologically active components of a subcritical CO2 extract of hot pepper fruits / / Medical and pharmaceutical journal "Pulse". - 2021. - Vol. 23. - No. 12. - Pp. 92-98]. In this regard, in order to ensure the safety of practitioners involved in the production of plant extracts, it is necessary to develop new methods to reduce the sublimation of capsaicin into the environment, thereby increasing both the safety level of working with alkaloid raw materials and the yield of extractive substances.

[0003] A method for obtaining capsaicinoids from the fruits of hot varieties of capsicum is known [USSR Author's Certificate No. 1622983, IPC A61K 36 / 81. Method for obtaining capsaicinoids: declared. 03 / 27 / 1989: published. 04 / 20 / 1995 / N.V. Popova, V.I. Litvinenko, T.P. Popova, A.S. Ammosov]. The method is carried out by extracting the fruits of hot varieties of capsicum with acetone and 90% aqueous acetone, purifying the evaporated extract with water, adding alkali, extracting the resulting mixture with ethyl acetate and ethyl alcohol, evaporating the organic phase, adding alkali to the resulting extract, purifying the mixture with petroleum ether and ethyl alcohol, and extracting the target product from the mixture with 10% ethyl alcohol in ethyl acetate in a mixture:extractant ratio of 1:(1.0...1.5). The yield is 58.5...62.5% of the capsaicinoids content in the raw material.

[0004] The disadvantages of this method are that its application relates only to medicine, the use of toxic substances as extractants, when working with which it is necessary to observe safety measures, including the use of personal protective equipment, in addition, the yield of extractive substances when using it is relatively low.

[0005] A method for obtaining an extract from the fruits of hot pepper of the genus Capsicum is known [Rudometova N.V., Kim I.S. Study of capsaicin extraction from the fruits of hot pepper of the genus Capsicum / / Scientific journal of NRU ITMO. Series "Processes and equipment of food production". - 2019. - No. 1. - P. 62-73]. The method is implemented as follows. Preliminary grinding of plant raw materials to a particle size of 1.5 ± 0.5 mm and its preliminary maceration in water with ultrasound exposure for one hour at a water ratio of 1: 5 and an ultrasound power of 128 W. Using a 70% aqueous solution of ethanol with a water ratio of 1:50 as an extractant and subsequent three-stage extraction, the duration of each stage is 30 min.If the specified parameters are met, according to the information provided by the authors of the method, the yield of capsaicin exceeds 99%, and the extraction time is reduced by half (from 5 to 2.5 hours), which makes it possible to choose this extraction method for preparing hot pepper fruit samples for the purpose of capsaicin analysis.

[0006] The disadvantage of this method is the low efficiency of using material resources, in this case the extractant, which is a 70% aqueous solution of ethanol, due to the hydromodulus of 1:50 recommended by the authors.

[0007] A known method for producing enriched vegetable oil with hot chili pepper extract [RU Patent No. 2680303, IPC C11B 1 / 00. Method for producing enriched vegetable oil with hot chili pepper extract: declared 06 / 14 / 2018: published 02 / 19 / 2019 / S.G. Popov]. The method involves selecting and preparing plant material from Capsicum hot peppers, which is subjected to forced drying, then grinding the dry peppers into a large fraction with a size in the range of 3 to 8 mm. Then, take one part of the vegetable oil, place the oil in a container and heat it to a temperature of 65°C, achieving uniform heating of the entire mass. After this, dry ground pepper is added to vegetable oil in an amount of 1 / 10 to 1 / 5 of a part, and extraction is carried out for 1 to 3 hours, maintaining the temperature in the range of 60 to 65°C.The invention makes it possible to obtain a food product enriched with capsaicin, possessing new taste properties, a pungent taste with a delayed effect, and also possessing biological activity due to the action of capsaicin and a long shelf life.

[0008] The disadvantage of this method is the relatively low solubility of capsaicin in vegetable oils, which may result in low intensity of mass exchange processes between the lipophilic components of plant cells and the oil extractant.

[0009] A common drawback of all the above-mentioned known methods is the lack of the ability to reduce the level of capsaicin sublimation into the environment, thereby making work with this alkaloid raw material extremely unsafe.

[0010] A method for extracting capsaicinoids from hot peppers with supercritical carbon dioxide is known [RU Patent No. 2750703, IPC A61K 47 / 58, A61K 36 / 81. Method for extracting capsaicinoids with supercritical carbon dioxide: declared 14.10.2020: published 01.07.2021 / D.S. Orlov, M.V. Vorobyov, N.K. Mukanova, A.A. Tsvetkov]. Extraction by the known method is carried out in two stages, wherein the first stage of the process uses carbon dioxide with the use of a co-solvent, which is distilled water, then the obtained extract is removed from the reactor, then the standard collector is replaced with a modified one, and the second stage is carried out, wherein liquefied carbon dioxide is used as a solvent for extraction in the second stage, after which the obtained extract is removed into the collector.The technical result consists in isolating two extracts: at the first stage, isolating an extract containing: capsaicinoids - 0.8...3.0% (of the total extract), essential oils - 0.5%, coloring agents - 72.0%, fatty oils - 1.0%, unidentifiable impurities - 20.0%; at the second stage, isolating an extract containing: capsaicinoids - 14...21% (of the total extract), essential oils - 23.0%, coloring agents - 14.0%, fatty oils - 43.0%).

[0011] The disadvantage of this method is the complexity and high cost of equipment for working under high pressure, which makes its use costly and often economically impractical, while the yield of extractive substances in this case can vary greatly depending on various factors of its implementation.

[0012] The closest solution in technical essence is the method for obtaining an extract of red hot pepper [USSR Author's Certificate No. 379258, IPC A23 1 / 28. Method for obtaining an extract of red hot pepper: declared. 16.08.1971: published. 20.04.1973 / Ya.S. Meerov, A.N. Katyuzhanskaya]. The method is implemented as follows. Hexane, liquid carbon dioxide, petroleum ether, acetone, alcohol, liquid butane or propane, etc. are usually used as a solvent. Extraction is carried out in two stages, in the first of which whole pods are processed. Since capsaicin is contained mainly in the pod shell, most of it is extracted in the first stage (the pods are not crushed to prevent the sublimation of capsaicin). The pods are then crushed and extracted again with the same solvent.Thus, the first stage of extraction primarily extracts capsaicin, essential oil, and coloring agents, while the second stage extracts the fatty oil, found primarily in the seeds, residual capsaicin, and the volatile components of the essential oil. The resulting extracts are then mixed.

[0013] The disadvantage of this method is the use of toxic liquids as an extractant, which leads to stages of its removal, and, accordingly, to the presence of residual amounts of the solvents used in the isolated extracts, which means that the purity and safety of the product is called into question.

[0014] Based on the analysis of known similar technical solutions, it was revealed that the technical problem in this area is the need to create safe methods for obtaining an extract from red hot pepper with a high content of capsaicinoids, by replacing the toxic extractant with a food analogue.

[0015] Technical result - obtaining an extract from red pepper with improved consumer characteristics and a high content of capsaicinoids.

[0016] In order to solve the technical problem and achieve the stated result in the method for obtaining an extract from red hot pepper, which includes the extraction of raw materials in two stages with grinding between the stages, wherein to obtain two different extracts based on the proportion of its constituent components, the extractive substances of fresh pepper are extracted with ethyl alcohol, and dried whole pods of red pepper are extracted with a 30% aqueous solution of ethyl alcohol, obtaining capsaicin, essential oil and coloring agents, and when extracting crushed raw materials - fresh or dried pepper, fatty oil, capsaicin residues and low-volatile components of the essential oil are obtained, while in order to obtain one extract containing all the extractive substances, including a high proportion of capsaicin content in it, at the second stage for extracting the crushed raw materials - fresh or dried pepper, the extract obtained at the first stage of extraction is used as a carrier of the extractant.

[0017] The invention will ensure the isolation of either one or two extracts without their subsequent mixing: the first extract includes mainly capsaicin, essential oil and coloring agents, and the second - fatty oil, contained mainly in the seeds, the remains of capsaicin and low-volatile components of the essential oil, in the case of isolation of one extract, according to the proposed method, in the second stage of extraction, the first extract is used, which is a carrier of a pure extractant and makes it possible to reduce the costs of solvents used in the proposed method.

[0018] The proposed method will ensure the production of an extract / extracts from red hot pepper without traces of chemicals, with a high content of capsaicinoids, with improved resource efficiency characteristics, while maintaining the effect of leveling the sublimation of capsaicin at all stages of the method, due to the replacement of the toxic extractant with ethyl alcohol or its mixture with water.

[0019] The technical result is achieved by the fact that the method for obtaining an extract from red hot pepper uses a Soxhlet extractor, and ethyl alcohol, which effectively dissolves capsaicin due to the presence of a hydroxyl group in its chemical structure, or a water-alcohol mixture that combines the hydrophobic properties of alcohol (dissolves non-polar parts) and the hydrophilic properties of water (interacts with polar groups), is used as an extractant, and since ethyl alcohol or its mixture with water are ingredients widely used in the food industry, the resulting extract or extracts can be used not only in the medical and perfumery and cosmetic industries, but also in the food industry.

[0020] The method is explained by the following examples of its implementation.

[0021] Example 1.

[0022] Using fresh raw materials.

[0023] The extraction is carried out in two stages. In the first, fresh whole red pepper pods with a moisture content in the range of 85–92% are processed. A sample of whole fresh peppers (8400 g, accurate to 10 g) is taken, divided into 7 portions, the separated portion is transferred to a Soxhlet apparatus (total volume 7.5 liters), and the extractive substances are extracted with 9600 g of ethyl alcohol, placed in a distillation still (total volume 25 liters) until the extractant in the extractor is visually transparent. The raw materials are then replaced, while the extractant remains, and this process is repeated until all raw materials in the sample are extracted. The resulting first extract is drained from the distillation still. Since capsaicin is found primarily in the pod shell, most of it is extracted in the first step (the pods are not crushed to prevent the capsaicin from sublimating).The pepper pods are then crushed, divided into three parts, and extracted again with a new batch of ethyl alcohol (9000 g) placed in a distillation still (total volume 25 liters) until the extractant in the still is visually clear. The resulting second extract is drained from the still. This produces two extracts: the first contains primarily capsaicin, essential oil, and coloring agents, while the second contains fatty oil, residual capsaicin, and low-volatile components of the essential oil (see Table 1).

[0024] Example 2.

[0025] Using dried raw materials.

[0026] The extraction is carried out in two stages. In the first, dried whole red pepper pods with a moisture content of no more than 14% are processed. A 1000 g sample of whole dried pepper is taken (accurate to 10 g), transferred to a Soxhlet apparatus (total volume 7.5 liters), and the extractive substances are extracted with 11,500 g of a 30% ethyl alcohol and water solution, placed in a distillation still (total volume 25 liters) until the extractant in the extractor can be visually considered transparent. The resulting first extract is drained from the distillation still. Then the pepper pods are crushed and extracted again with a new batch of 10,000 g of a 30% ethyl alcohol and water solution until the extractant in the extractor can be visually considered transparent. The resulting second extract is drained from the distillation still.In this way, two extracts are obtained, the first of which contains mainly capsaicin, essential oil and coloring agents, and the second - fatty oil, remains of capsaicin and low-volatile components of the essential oil (see Table 1).

[0027] Example 3.

[0028] Using either fresh or dried raw materials.

[0029] The first stage of extraction is carried out as shown in Examples 1 and 2, depending on the raw material used. The only difference is the decanting of the resulting extract, which will serve as a carrier for the extractant selected based on the raw material. Next, the plant material is crushed, loaded into a Soxhlet extractor, and further extraction is carried out until the extractant in the extractor is visually clear. The resulting extract is decanted from the distillation still. This results in a single extract containing all extractive substances, namely capsaicin, essential oil, coloring agents, fatty oil, and the low-volatile components of the essential oil (see Table 1).

[0030] The approximate chemical composition of the obtained extracts is given in Table 1.

[0031]

[0032] As can be seen from Table 1, the use of the proposed method, in comparison with the known one, gives similar results, while it is safer to perform, since a food extractant is used in its use.

[0033] Positive effect:

[0034] - the proposed method allows one to obtain from red hot pepper two different extracts based on the proportion of the components included in it, or one extract with a high proportion of capsaicin content in it, while saving, for this version of the application of the proposed method, on the amount of extractant used by almost 2 times, while maintaining the effect of leveling the sublimation of capsaicin at all stages of the implementation of the method, due to the replacement of the toxic extractant with ethyl alcohol or its mixture with water.

Images