RU2015694C1 - Method for production of dry hydrophytoconcentrates - Google Patents

Abstract

FIELD: cosmetics. SUBSTANCE: method develops a radically new process of complex processing of vegetable raw materials and byproducts of food industry in order to produce biologically-active substances. Method reduces the time required for production, improves the quality of dry additions by the use of adsorbents constituted by aqueous solution of a mixture of structuring and surface-active substances or an aqueous solution of structuring substances and mineral additions. Structuring substances are colloids such as carboxymethylcellulose, sodium carbomethylcellulose (NaCMC), gelatine, starch paste, paste-like mixtures of groats. Surface-active materials are sodiumlaurylsulfate, oleate, stearate, diethanolamides; mineral additions are chalk, kaolin, sodium chloride, depending on the use of powdered hydrophytoconcentrate. EFFECT: higher efficiency. 9 cl, 6 tbl

Description

 The invention relates to cosmetics and relates to a method for the production of biologically active additives - powder hydrophytoconcentrates with a wide spectrum of action for inclusion in cosmetic products.

 There are various methods for the production of herbal supplements that are carriers of biologically active substances, aroma, color, taste, etc.

 Known methods for producing dry plant biologically active additives by fine grinding using in preparations for brushing teeth, drugs that accelerate hair growth, in cleansing preparations, in drugs to accelerate growth and strengthen hair.

 Closest to the proposed method, used to obtain dry extracts from medicinal plants, which can be used in the manufacture of cosmetic products as biologically active substances, fragrances (in body washes and bath foams), which consists in preparing an extract, thickening it in a vacuum apparatus to a thick extract, vacuum-drying the extract to dryness and grinding, sifting the obtained extract (see source).

 Plant materials are dried, crushed, and extracted with water to extract water-soluble components. Water extracts containing ballast substances (pectins, mucus, starch, etc.) are subjected to additional processing - they are clarified by boiling and alcohol. Extracts cleaned from ballast substances are passed to thickening.

In order to preserve the active ingredients extracted from the crude drug (thermolabile substances - alkaloids, vitamins, glycosides, hormones), evaporating the water extract is carried out at a temperature of about 45 ^{° C,} a residual pressure of about 0.1 kg / cm ^2.

 Then the condensed water extracts are subjected to drying in a drying apparatus. Two types of dryers are used: the substance to be dried is located directly on the heated surface; drying is carried out by the flow of heat carrier gas, which is air. After drying, the extract is ground and sieved.

 However, the production process of dry extracts according to the described method is very long, requires large expenditures of heat, electricity, water. The dry extract obtained as a result has low biological activity, a narrow range of applications due to the large losses of aromatic substances, natural dyes and thermolabile components. This is explained by repeated long-term heat treatments of the obtained aqueous extracts, as a result of which the initial composition of the biologically active substances, color and smell change.

 Thus, the existing scheme for the production of dry extracts from plant materials cannot provide a high-quality product, the use of which, as a source of biologically active substances, natural dyes and flavorings, would guarantee high quality products using dry extracts.

 The invention solves the problem of developing a fundamentally new technology for the integrated processing of plant materials - medicinal, aromatic, essential oil, fruit and vegetable and by-products of food production in order to obtain high-quality powder hydrophytoconcentrates. Reducing the time of the process of preparing dry extractive substances is achieved by using adsorbents and minerals that provide the natural introduction of hydrophytoconcentrates in cosmetic products.

 The goal is achieved in that an aqueous solution of structure-forming substances or an aqueous solution of a mixture of structure-forming and surface-active substances is used as an adsorbent to obtain powder hydrophytoconcentrates. Moreover, the introduction of these solutions is carried out before drying and a mixture of structure-forming substances and water is taken in the ratio, wt.%: (7.5-15.0) :( 92.5-85.0). A mixture of structure-forming substances, surfactants and water is taken in the ratio (1-5) :( 0.5-2.5) :( 98.5-92.5).

 For the purpose of uniformity of the introduction of powder hydrophytoconcentrates, the bulk density is adjusted by introducing mineral substances before or after drying, in the amount of 3-10% of the composition of the mixture fed to the drying, depending on the type of raw material used and the purpose of the finished product.

 Colloids - carboxymethyl cellulose (CMC) or sodium carboxymethyl cellulose (Na-CMC), gelatin, gelatinized starch, gelatinized mixture of cereal raw materials are used as structure-forming substances; as surfactants - sodium lauryl sulfate, oleate, stearate, diethanolamides FFA; as mineral additives - chalk, kaolin, sodium chloride - depending on the object of use of powder hydrophytoconcentrate.

 With the appropriate introduction of a mixture of adsorbents, minerals, they provide high-quality powder hydrophytoconcentrates with a natural aroma, color and native complex of biologically active substances.

 The method of obtaining powder hydrophytoconcentrates consists of the following stages: preparation of plant materials; obtaining a hydrophilic fraction; mixing the hydrophilic fraction with the adsorbent; homogenization of the mixture; drying, for example, in a pseudo-boiling, vibro-boiling, boiling, in a fluidized bed inert carrier; obtaining a conditioned product.

 Preparation of plant materials consists in drying plants, their grinding, weighing and transfer to extraction. Fruits, berries and other juicy raw materials are sorted, washed and served for extraction. If waste or by-products of food production are used as raw materials, they are subjected to additional grinding and transferred to extraction.

 Water extraction is carried out in extractors with a stirrer and a heating jacket.

 To select the most favorable conditions for the extraction process, factors that have a maximum effect on the yield of extractive substances and the amount of biologically active substances are determined. Such factors include: the number of stages of the extraction process, the phase ratio (feed: solvent), extraction time and temperature. Values of factors are given in table. 1. In addition, the individual characteristics of the raw materials were taken into account (the nature of the main biologically active substances, the object of use, which component is needed in the maximum quantity).

 To study the extraction process and select the optimal conditions used mathematical design of the experiment (table. 2). Chamomile was extracted, extraction was carried out with an acidified aqueous solution with pH = 4-5 (to create optimal conditions for the transition of chamazulenes to azulene).

 The efficiency of the extraction process was assessed by the yield of extractives and the content of prochamazulenes.

As a result of a series of experiments, the optimal modes of water extraction were determined: the number of stages of the extraction process 2; total extraction time 90 min; the extraction temperature is 60-80 ^{° C,} the phase ratio of 1: 5-1: 10.

 The selected mode provides a high content of biologically active substances while maintaining their quality and a high yield of extractive substances. The resulting aqueous extracts (hydrophilic fraction of plant materials) contain 3-20% solids.

 With increasing temperature and extraction time, the yield of extractive substances increases, but the quality of biologically active substances (in this case, the content of prochamazulenes) deteriorates.

 An important technological operation is the drying of the hydrophilic fraction of vegetable raw materials obtained by pressing juicy raw materials or in the process of water extraction. The type of drying during dehydration of plant products significantly affects the safety of substances that determine the biological value of plant materials (vitamins, organic acids and their salts, amino acids, pectin and polyphenolic compounds, sugars, plant pigments, etc.), and ultimately, the quality finished product.

 Conventional and vacuum drying of the hydrophilic fraction is impractical due to the high energy costs, the duration and multi-stage process, as well as the complexity of the input, use of dry extractive substances in cosmetic products, color changes, and odor.

 Known drying in a fluidized bed of inert bodies - melange, gelatin, protein-containing solutions, etc. Due to the specific features of the chemical composition of these substances - a significant content of heat-resistant and flow-giving substances - these products do not require special conditions for the drying process. In addition, the above substances do not show adhesion to the fluoroplastic, the surfaces of the drying chamber, cyclone, pipelines.

 Fluidized bed drying of an inert material to obtain powdered dry extracts, despite the advantages - good loosening of the dried material; lack of overheating and temperature equalization in the volume of the layer due to intensive mixing; an increase in the contact surface of the dried material with a drying agent and intensive evaporation of moisture; preventing the formation of lumps and grinding particles with inert bodies does not solve the problem of obtaining a high-quality final product. This is due to specific features of the chemical composition of the hydrophilic fraction of plants. In the process of drying in a stream of hot air, it quickly heats up and slowly releases the moisture contained in it, because has sufficiently strong energy bonds with moisture. In addition, as a result of the processes of dehydration, polycondensation, caramelization and others, there is a change in physicochemical properties and an increase in adhesive properties. All this affects the appearance, aroma and other factors of the biological value of the final product.

 The aqueous extract fed to the drying unit adheres to the inert carrier and the walls of the drying chamber, caramelizes, the fluidized fluidized bed settles, and the drying process itself becomes impracticable.

 To obtain highly effective, powder hydrophytoconcentrates from various plant objects, drying of the hydrophilic fraction of the raw material using adsorbents — polystructural substances and mixtures of them with surface-active substances (SAS) is proposed.

 In order to study the effect of various polystructural substances and their mixtures with surfactants on the stability of the quality of powder hydrophytoconcentrates, a series of experiments was carried out using mathematical planning on a simplex.

 The drying process was evaluated by the ability of a dry hydrophytoconcentrate to dissolve in water, i.e. on the recoverability of the final product.

 The matrix, experimental design and research results are given in table. 3.

 Based on the results of the studies, the composition - property diagrams were constructed, the optimal version of the adsorbent used for drying the hydrophilic fraction of plant materials was determined. The best option is a mixture of a hydrophilic fraction of plant materials and polystructural substances or a hydrophilic fraction, polystructural substances and surfactants.

 Adsorbents in the drying process were used: to create the possibility of the drying process; to preserve biologically active substances, organoleptic properties and color; to give the powder flowability; to obtain a renewable product with hydrophilic properties; for obtaining powder hydrophytoconcentrates of the intended purpose, because the composition of the adsorbent may vary depending on the purpose of use of the final product - for specific types of cosmetic products.

 Colloids, substances of plant and animal origin, which form colloidal solutions with water and can be used to form gels, increase the viscosity of solutions and emulsions as stabilizers, were used as structure-forming substances. CMC-Na, CMC, gelatin, gelatinized starch, gelatinized cereal mixes were tested.

 Surfactants give stability to disperse systems, can act as solubilizers, thickeners emulsions, stabilizers of quality, showing bactericidal properties.

 However, when the adsorbent (colloids, a mixture of colloids and surfactants) is directly introduced into the hydrophilic fraction, it takes more time for the structure-forming substances to swell than the hydrophilic fraction can be stored. At the time of colloid swelling, water extracts, squeezed fruits, etc. sour, ferment, i.e. not subject to further processing.

 Therefore, it became necessary to prepare an aqueous mixture of adsorbents in advance. To determine the optimal ratio of these ingredients, a mathematical planning matrix on a simplex was compiled and experiments were carried out in triplicate using each variant of the mixture when drying the hydrophilic fraction of plants. For example, an aqueous extract from a raw mixture of chamomile, seeds, carrots and rice flour. In this case, the effectiveness of the obtained aqueous mixture of adsorbents was assessed by the quality of drying, by the time of recoverability of the finished product, and by the content of prochamazulenes as the most valuable biologically active substances (Table 4).

 It has been established that the maximum amount of prochamazulenes is contained in a hydrophytoconcentrate obtained by using an aqueous mixture of structure-forming and surface-active substances as an adsorbent at a ratio, wt. %: structure-forming substances: surfactant: water - (1-5) :( 0.5-2.5): (98.5-92.5).

 Depending on the type of raw material and the finished product, it is possible to use as an adsorbent an aqueous solution of structure-forming substances. In order to determine the optimal composition of this solution, the ratios of water and colloids in the range of 1: 100 and 100: 1 were analyzed.

 The best composition of the aqueous mixture is determined by the ratio of structure-forming substances: water (7.5-15) :( 92.5-85).

 The same studies were carried out when drying juices and other types of aqueous extracts with different contents of extractive substances. These studies have confirmed the effectiveness of using the selected optimal ratio of structure-forming, surfactants and water when drying various types of hydrophilic fractions of plants with a dry matter content of 3 to 20%.

 With a low content of extractives in the hydrophilic fraction, it becomes necessary to use an adsorbent enhancer - mineral substances.

 In order to determine the optimal composition of the mixture of the hydrophilic fraction of the plant and the aqueous mixture of the adsorbent, a series of experiments was carried out to find the ratio of the hydrophilic fraction of the plant and the adsorbent, and when using mineral substances, the hydrophilic fraction of the plant, adsorbent and mineral substances.

 In the first series of experiments, the ratios of the hydrophilic fraction of plants and the adsorbent were analyzed. The best composition of the mixture fed to drying, in this case, is (by the content of the main biologically active substances), wt.%: Hydrophilic fraction of the plant 25-45; adsorbent 55-75.

 To select the optimal composition of the mixture fed to drying, using mineral substances, a series of experiments on the matrix were carried out (Table 5).

 As a result of a series of experiments, it was found that the maximum yield of hydrophytoconcentrates with a high content of biologically active substances is guaranteed by feeding to the mixture a mixture consisting of, wt.%: The hydrophilic fraction of the plant 20-40; adsorbent 50-77; mineral substances 3-10.

 In some cases, if it is necessary to evenly distribute powdered hydrophytoconcentrates in certain environments (toothpastes, powders, dry cosmetics), it is advisable to introduce the same minerals that are components of these agents into the powder hydrophytoconcentrate in an amount of 3-10% after drying.

 After mixing in a container with a stirrer and heating the hydrophilic fraction of the plant with adsorbent and minerals (if they are used), the resulting composition is fed to homogenization, which is carried out in the homogenizer for 15-20 minutes. Then the homogenized mixture is fed to a dryer.

 Obtaining a homogeneous system supplied to the drying mixture is an important condition for this technical solution. A decrease in homogeneity significantly affects the drying process - thermoplastic substances of plant extracts that do not interact with the adsorbent are caramelized, stick to the walls of the drying chamber and an inert carrier, which makes it impossible to continue the process.

 In the process of homogenization of the adsorbent with the hydrophilic fraction of the plant and subsequent temperature exposure during drying, complex physicochemical changes occur due to the adhesive effect, diffusion phenomena, the chemical interaction of the substances of the plant extract (hydrophilic fraction) with the adsorbent substances, dehydrogenation, decarboxylation, polycondensation, aer and thermal oxidation of chemical compounds of the drying object and many other processes. All these processes are linked into a single, very complex process of heat and mass transfer.

 The presence of an affinity between extractive substances of plant materials and adsorbents that promote the formation of adhesive interaction during homogenization and drying allows us to obtain a fundamentally new product that is homogeneous and does not separate into the original components. It is the homogenization of the mixture of the adsorbent and the hydrophilic fraction that allows you to save the aroma in a dry product. Retention of aroma substances is a complex, poorly studied physicochemical process, which in this case is apparently due to the formation of a dense product film during homogenization and the initial stage of the drying process, which is well permeable to water vapor and poorly permeable to aroma substances, due to differences their diffusion coefficients.

 Thus, the use of drying a hydrophilic fraction in a fluidized bed of inert bodies without mixing the hydrophilic fraction with the developed target adsorbent and homogenizing the mixture makes it impossible for the process to proceed due to caramelization of the product, its sticking to an inert carrier and walls of the drying unit. Drying is carried out in a pseudo-boiling layer of inert material in a drying plant of type A1-FMU.

 The finished product - powder hydrophytoconcentrate - is fed to the packaging and storage. If the introduction of mineral substances is required - in a container with a mixer for granular masses, where there is a uniform introduction of mineral substances into the finished product.

Studies of the quality of the obtained samples of powder hydrophytoconcentrates from mixtures of medicinal, spicy aromatic, essential oil raw materials, juice products and waste products, waste after CO ₂ extraction, secondary food production products showed a significant improvement in the quality of “dry” extractive substances obtained by the proposed method in comparison with prototype. The content of biologically active substances increased due to the conservation of thermolabile components, natural dyes and aroma carriers. The use of a mixture of adsorbents (structure-forming substances and surfactants) or structure-forming substances significantly accelerated and simplified the drying process of hydrophilic fractions.

 The use of a scientifically based ratio of structure-forming surfactants and water in the process of producing powder hydrophytoconcentrates enhanced the bactericidal properties of surfactants, as a result of which the final product does not require additional processing in order to increase the shelf life. This ratio of adsorbent and hydrophilic fraction helps to obtain the final product in a form convenient for inclusion in any cosmetic products, household chemicals, etc. During storage, hydrophytoconcentrates do not cake, do not lose their original color and aroma.

 The finished product has high biological activity and ease of introduction into any cosmetic products, household chemicals. Those. The developed method for producing powder hydrophytoconcentrates for cosmetics guarantees the production of such a product that can be used as a source of natural dyes, biologically active substances, and flavoring. In addition, the proposed method differs from the traditional significant savings in electricity, steam, water and time.

PRI me R 1. Hydrophytoconcentrate for cosmetic creams and toothpastes. 15.6 kg of plant material consisting of calendula, rice waste, carrot seeds in a ratio of 0.7: 0.2: 0.1 and 162.2 l of water are loaded into the extractor. Mix, insist 15 minutes at t = (60 ± 5) ^o C and cool for 30 minutes. The mass is squeezed, the extract l is filtered off and again fed to the extractor loaded with 15.6 kg of fresh raw materials. 47.1 liters of water are added and insisted for 15 minutes at t = (60 ± 5) ^o C and 30 minutes under cooling. The mixture is squeezed, the extract II is filtered.

 Preliminarily, 4.1 kg of Na-CMC is dissolved in 131.1 l of water. The resulting Na-CMC solution is mixed with 2.0 kg of PEG-400 oleate and the finished extract II is poured. The mixture is homogenized. The resulting finely divided mixture is dried in a vibro-boiling layer of inert material on an A1-FMU dryer.

PRI me R 2. Hydrophytoconcentrate for toothpastes. The extractor was charged with 9.4 kg of chamomile plant raw material and 97.8 l of acidified water having a pH = 5. The mixture is stirred, insist 15 min at t = (60 ± 5) ^{° C} and 30 min at cooling. The mass is squeezed, the extract l is filtered and again fed to the extractor for 9.4 kg of fresh raw materials. Add 30.8 liters of water, insist 15 minutes at t = (60 ± 5) ^o C and 30 minutes upon cooling. The mixture is squeezed, the extract II is filtered.

 Preliminarily, 1.6 kg of Na-CMC is dissolved in 50.6 l of water. The resulting Na-CMC solution was mixed with 0.8 kg of sodium lauryl sulfate, extract II was added, and 6.2 kg of chalk was added. The mixture is homogenized. The resulting mixture is dried in a "vibro-boiling" layer of inert material on an A1-FMU dryer.

PRI me R 3. Protein hydrophytoconcentrate for a cosmetic mask. 6.2 kg of husk of sunflower seeds and 84.6 l of a 10% aqueous solution of sodium chloride (NaCl) are loaded into the extractor. Mix, insist 15 minutes at t = (60 ± 5) ^o C and cool for 30 minutes. The mass is squeezed, the extract I is filtered off and again fed to the extractor for 6.2 kg of fresh raw materials. Add 14 liters of water and insist 15 minutes at t = (60 ± 5) ^o C and 30 minutes upon cooling. The mixture is squeezed, the extract II is filtered.

10 kg of rice crusher are loaded into a boiler with a shirt and a stirrer and 100 l of water are poured. Cook rice for 35-40 minutes until cooked at t = 100 ^o C. At the end of cooking, rice with rice broth is homogenized. Extract II was poured to the resulting mass and homogenized again.

 The finely dispersed mixture is dried in a vibratory boiling layer of an inert material of the A1-FMU dryer.

 PRI me R 4. Hydrophytoconcentrate quince for cosmetic milk. The juice obtained from quince is mixed with a previously prepared solution of Na-CMC. To prepare this solution, 4.7 kg of Na-CMC and 142.1 l of water are taken. The resulting Na-CMC solution is mixed with 2.3 kg of PEG-400 oleate and 100 l quince juice is added. The mixture is homogenized. The resulting finely divided mixture is dried in a vibro-boiling layer of inert material on an A1-FMU dryer.

 Other examples of the preparation of various types of hydrophytoconcentrates are given in table. 6.

 The proposed technology allows to obtain new powder products with a high concentration of hydrophilic biologically active substances in their native state; highly porous, flocculent structure providing fast solubility and manufacturability; good flowability; the possibility of long-term storage; Convenience in dosage and transportation.

 Hydrophytoconcentrates have a pleasant natural aroma, characteristic of the feedstock, have biological activity.

 The developed technology involves the use of domestic mass-produced equipment and high production efficiency.

 The production of hydrophytoconcentrates will allow waste-free processing of expensive plant materials and expand the range of cosmetic products, household chemicals by creating powder biocosmetics.

 Implementation of the developed technology is carried out at the enterprise of the experimental facility "Central" and the small enterprise "BIAM" in Krasnodar.

Claims (7)

 1. METHOD FOR PRODUCING DRY HYDROPHYTHO CONCENTRATES by grinding the raw material, isolating the hydrophilic fraction and drying, characterized in that the hydrophilic fraction of the raw material is obtained by extraction or extraction with aqueous solutions with a pH of 5-10 to a dry matter content of 3-20%, then the hydrophilic fraction of the raw material is mixed with the adsorbent , the mixture is homogenized.  2. The method according to claim 1, characterized in that the extraction is carried out with water or an aqueous solution of acids, alkalis or salts.  3. The method according to claim 1, characterized in that an aqueous mixture of structure-forming substances is used as an adsorbent with a ratio of structure-forming substances and water, wt.%: (7.5 - 15): (92.5 - 85).  4. The method according to claim 1, characterized in that as an adsorbent use an aqueous mixture of structure-forming and surface-active substances with a ratio of structure-forming substances, surfactants and water (1 - 5): (0.5 - 2.5) : (98.5 - 92.5). 5. The method according to p. 1, characterized in that the mixture supplied to the drying has a composition, wt.%:
Hydrophilic fraction of raw materials 25 - 45
Adsorbent 55 - 75
6. The method according to p. 1, characterized in that with the adsorbent additionally injected minerals in an amount of 3 to 10% of the composition of the mixture fed to the drying. 7. The method according to claim 6, characterized in that the mixture fed to the drying has a composition, wt.%:
Hydrophilic fraction of raw materials 40 - 20
Adsorbent 50 - 77
Minerals 10 - 3
8. The method according to claim 6, characterized in that the mineral substances are introduced into the product after drying in an amount of 3 to 10%.  9. The method according to PP.3 and 5, characterized in that the structure-forming substances use CMC or CMC-Na colloids, or gelatin, or gelatinized starch, or gelatinized cereal raw materials, as surface-active substances - sodium aluryl sulfate or oleate, or stearate or FFA diethanolamides, chalk or kaolin, or sodium chloride are used as mineral additives, depending on the object of using powder hydrophytoconcentrate.

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