RU2668517C1 - Method for producing propylene glycol extract of shilajit - Google Patents

Abstract

FIELD: technological processes.SUBSTANCE: invention relates to a method for processing natural shilajit-containing feedstock, namely to a method for producing a propylene glycol extract of shilajit. Method for producing a propylene glycol extract of shilajit comprising extracting a purified shilajit-containing feedstock with an extractant being propylene glycol or a mixture of propylene glycol and water, under certain conditions, followed by filtration of the extract.EFFECT: described method provides an extract with a high extractable substance content and increased resistance to microbiological contamination.1 cl, 2 tbl, 14 ex

Description

The invention relates to methods for processing natural mummy-containing raw materials, in particular, to methods for producing propylene glycol extracts of mummy - the sought-after natural components of cosmetics and perfumery products, household chemicals and detergents.

Mummies are currently used in medicine both in their native form and in the form of various dosage forms (ointments, tablets, suppositories, etc.) As a rule, mummy-containing raw materials contain up to 50% mummy in a resinous form. To isolate mummies from natural raw materials, as a rule, multistage aqueous extraction is used, followed by filtration, drying and obtaining dry extracts, which are used in dosage forms.

A known method of producing aqueous extracts of mummies, which consists in pre-grinding the mummified rock to a particle size of not more than 1 mm, extraction with distilled water, repeated filtration and subsequent evaporation of the filtrate to obtain an extract containing not more than 3.5% water, which are then tabletted and packaged ( patent RU 2001618 A61K 35/00, published on 10/30/1993)

There is also a method of producing mummy extracts from mummy-containing raw materials by countercurrent dissolution in water to achieve a solution density of 1.05-1.075 g / cm ³ , filtering and evaporating the resulting solution followed by tabletting (patent RU 2102989, A61K 35/00 publ. 01.27.1998 g.).

There is also a method of producing mummy extracts by extraction of crushed raw materials with distilled water in a rotary pulsation extractor, followed by removal of water in a rotary film dryer (patent RU 2114626 A61K 35/12 publ. 07/10/1998).

There is also known a method of obtaining a bioactive extract based on mummified materials. The method involves the following stages: pre-soaking in distilled water, ultrasonic treatment of the solution, settling and separation of the undissolved fraction by decantation, ultrafiltration, freeze-drying to a content of at least 95% mass fraction of solids, disinfecting the resulting product with mercury germicidal lamps and vacuum packaging of the product (Patent RU 2164411 A61K 35/00 publ. 03/27/2001).

However, the solid state of mumiye extracts limits the possibility of their use in modern products of household chemicals and the cosmetics and perfumery industry with a low water content, and also increases the duration of the technological process of manufacturing cosmetic and perfumery products due to the need for preliminary dissolution of solid extracts in the right solvent, filtering the resulting solution, which also leads to higher prices for the target products. In addition, not every company has such an opportunity. Due to the low microbiological purity and short warranty periods of water extracts of mummies, their use in the manufacture of cosmetics and perfumes is also very limited.

It is important to note that water-alcohol extracts of natural raw materials, previously widely used, are now extremely rarely used in the formulations of cosmetic and perfumery products due to the fact that they belong to the class of flammable liquids and require special conditions of transportation, storage and use. Moreover, after the introduction of excise taxes on alcohol-containing solutions, including water-alcohol extracts, the production of the latter in Russia has risen sharply. It should also be noted that there is such a problem with the use of water-alcohol extracts as their exfoliating effect in cosmetic and hygienic detergents, which is especially noticeable in formulations containing pearlescent and thickening components [M.Yu. Pletnev. Cosmetic and hygienic detergents. M .: "Chemistry", 1990]. An alternative to water-alcohol extracts would be water-glycerol extracts, however, due to the high viscosity of glycerol and low diffusion coefficients, the rate of mass transfer processes and the degree of extraction of active substances is extremely small. In addition, the high viscosity of water-glycerin extracts creates technological problems in their production and use in the formulations of cosmetic products.

Closest to glycerin in its chemical structure is propylene glycol, which still has bactericidal activity. In cosmetics, propylene glycol is used as a water-retaining agent, but having a lower viscosity (density comparable to water), it is also an excellent enhancer - a substance that helps the active substances from cosmetic products to easily penetrate the protective layer of the skin. All this makes propylene glycol extracts of mummies very attractive for use in household products.

The objective of the invention is the development of a method for producing liquid extracts of mummy for use in cosmetic and perfumery products and household chemicals.

EFFECT: propylene glycolic extracts of mummy that maintain microbiological purity during the guaranteed storage period (up to 12 months) with a yield of extracted substances of at least 60%.

The technical result is achieved by the proposed method for producing propylene glycol extracts of mummy, in which the extraction of the purified mummy-containing raw materials is carried out with propylene glycol or a mixture of propylene glycol with water at a mass ratio of mummy-containing raw materials: extractant = 1: (10-20) for 2-4 hours at a stirring speed of not more than 40 rpm and temperature not exceeding 35 ° C, followed by filtration of the extract. A mixture of propylene glycol and water contains not more than 75 mass. % water. When the content in the extractant is more than 50 mass. % the Microker IT preservative is introduced into the extract in an amount of 0.01-0.05% by weight of the extract (a special case of the method).

For extraction, we used mummy-containing raw materials according to TU 9377-003-21454432-14 in the form of a thick dark brown resin with a moisture content of 20%, propylene glycol according to TU 6-09-2434-81 or according to TU 2422-059-05766801-97. Microker IT (a mixture of methylisothiazolinone and methylchloroisothiazolinone) is a preservative manufacturer Thor GmbH, Germany.

The filtration of the extract was carried out by known means, for example, through a paper or fabric filter.

Stirring at a speed of over 40 rpm./minutes leads to the fact that part of the impurities contained in the feedstock is transferred to the extract in the form of an emulsion contaminating the target product, in addition, considerable time is required to separate the emulsion, which is technologically and economically not feasible.

When extraction is less than 2 hours, a high degree of extraction of the extracted substances is not achieved, more than 4 hours is not economically feasible.

Raising the temperature above these parameters is not recommended, since it leads to a decrease in the yield of the target product due to hydration and hydrolysis of the beneficial components of the mummy at higher temperatures.

The ratio of the initial mummy-containing raw material and extractant below G. 10 is technologically impractical, because part of the product being extracted is subsequently separated from the extract.

The ratio of the initial mummy-containing raw material and extractant above 1:20 is not economically feasible due to a decrease in the concentration of extracted components of the mummy, which leads to the necessity of introducing a larger amount of extract into the formulations of cosmetics and household chemical products and, accordingly, to the cost of cosmetic products.

It is known that the demand for extracts is determined by two factors: biological value and resistance to microbiological pollution. The biological value of plant raw material extracts is determined by the quantitative content of biologically active substances extracted from mummy-containing raw materials, in this case it will be determined by the amount of non-removable (dry) residue from the propylene glycol extract, determined in accordance with Technical Specifications TU 9154-010-02700055-2002 letter A as amended 1,2,3,4.5. By microbiological purity, plant extracts must meet the sanitary requirements of SanPin 1.2.681-97; MUK 4.2.801-99, GF XII, part 1, sec. 32 (OFS 42-0067-07). Determination of the microbiological purity of the obtained extract was carried out in accordance with the Methodological Instructions of MUK 4.2.801-99 "Methods of microbiological control of perfumes and cosmetics."

The inventive method is illustrated by the following examples:

Example 1. In a glass extractor equipped with a reflux condenser, a mechanical stirrer and a thermometer, 50 g of mummified material was charged and 1000 g of propylene glycol was added. The mixture is slowly stirred for 4 hours, periodically including a stirrer (rotation speed of not more than 40 rpm.) At a temperature of no higher than 35 ° C. After cooling to room temperature, the solution is filtered using a paper or fabric filter. The obtained extract of dark brown color is analyzed for standard quality indicators and microbiological purity. The results of the analysis are presented in tables 1 and 2. The yield of extractables (61.0%) is determined by the amount of non-removable (dry) residue.

Example 2. In a reaction vessel, 50 g of mummified material was charged and 500 g of propylene glycol was added. Further, the process is carried out analogously to example 1. The yield of extractables is 66.75%.

Example 3. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant containing 950 g (95%) of propylene glycol and 50 g (5%) of distilled water were added. Further, the process is carried out analogously to example 1. The yield of extractable substances 71.5%.

Example 4. In the reaction vessel, 50 g of mummified material was charged and 500 g of extractant containing 475 g (95%) of propylene glycol and 25 g (5%) of distilled water were added. Further, the process is carried out analogously to example 1. The yield of extractable substances 72.0%.

Example 5. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant containing 750 g (75%) of propylene glycol and 250 g (25%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 3 hours. The yield of extractables is 83.0%.

Example 6. In the reaction vessel, 50 g of mummified material was charged and 500 g of extractant containing 375 g (75%) of propylene glycol and 125 g (25%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 3 hours. The yield of extractable substances is 81.0%.

Example 7. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant containing 500 g (50%) of propylene glycol and 500 g (50%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 3 hours. The Microker IT preservative is introduced into the finished extract in an amount of 0.01% by weight of the extract. The yield of extractable substances is 97.25%.

Example 8. In the reaction vessel, 50 g of mummified material was charged and 500 g of extractant containing 250 g (50%) of propylene glycol and 250 g (50%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 3 hours. The Microker IT preservative is introduced into the finished extract in an amount of 0.01% by weight of the extract. The yield of extractables is 96.75%.

Example 9. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant containing 250 g (25%) of propylene glycol and 750 g (75%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractables is 98.75%.

Example 10. In the reaction vessel, 50 g of mummified material was charged and 500 g of extractant containing 125 g (25%) of propylene glycol and 375 g (75%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractable substances is 98.5%.

Example 11. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant containing 50 g (5%) of propylene glycol and 950 g (95%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractable substances is 99.25%.

Example 12. In the reaction vessel, 50 g of mummified material was charged and 500 g of extractant containing 25 g (5%) of propylene glycol and 475 g (95%) of distilled water were added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractables is 98.75%.

Example 13. In the reaction vessel, 50 g of mummified material was charged and 1000 g of extractant — distilled water — was added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractable substances is 99.75%.

Example 14. In the reaction vessel, 50 g of mummified material was loaded and 500 g of extractant — distilled water — was added. Next, the process is carried out analogously to example 1. The extraction time is 2 hours. The preservative Microker IT is introduced into the finished extract in an amount of 0.05% by weight of the extract. The yield of extractable substances is 99.5%.

The extracts obtained in accordance with examples 1-14 are transparent dark brown liquids, the quality indicators of which are given in table 1, meet the requirements of TU 9154-010-02700055-2002 "Propylene glycol extracts, letter A" with changes 1, 2,3,5,5 (for water-propylene glycol extracts) and TU 9154-014-12967730-2006 "Water extracts of plant materials, letter A" (for water extracts).

As follows from the data in table 1, all extracts obtained (examples 1-14) have a yield of extractable substances of at least 60% (61.0 - 99.75). Microbiological purity (Table 2) of water-propylene glycol extracts with a water content of not more than 50%, both with the use of a preservative in an amount of 0.01%, and without the use of a preservative, remains during the warranty period - 12 months (examples 1-8). With a further increase in the water content in the extracts, their microbiological purity for 12 months is preserved only when the preservative content is not less than 0.05% (examples 9.10). In aqueous extracts (examples 13.14) without a preservative, microbiological purity is preserved for no more than 5 days, with the use of 0.05% preservative for no more than 30 days. Thus, the claimed technical result is achieved in cases where the extractant is propylene glycol or a mixture of propylene glycol with water containing not more than 75 mass% of water.

The inventive method for producing propylene glycol extracts of mummies provides extracts with a high content of extractable substances (up to 98%) with increased resistance to microbiological contamination (up to 12 months from the date of manufacture) while maintaining organoleptic and physico-chemical quality indicators corresponding to current regulatory documentation.

Note: * - Microker IT preservative was introduced in an amount of 0.01% by weight of the extract

** - introduced Microker IT preservative in the amount of 0.05% by weight of the extract

Claims (2)

1. A method of obtaining propylene glycol extracts of mummies, including the extraction of purified mummies-containing raw materials with an extractant representing propylene glycol or a mixture of propylene glycol with water containing not more than 75 mass. % water, with a mass ratio of mummies containing raw materials: extractant = 1: (10 - 20) for 2-4 hours at a stirring speed of not more than 40 rpm and a temperature of no higher than 35 ° C, followed by filtration of the extract. 2. A method of producing propylene glycol extracts of mummy according to claim 1, wherein when the content in the extractant is more than 50 mass. % in the extract is introduced the preservative Microker IT in an amount of 0.01-0.05% by weight of the extract.