RU1790598C - Method for production of extract from essential oil vegetable juice - Google Patents

Abstract

The invention relates to the essential oil industry and relates to the extraction of extractives from plant materials. In order to increase the yield of alcohol and fat soluble substances, the extraction is carried out with environmentally friendly ethyl alcohol and methylene chloride in two stages. In the first stage, the feed is ground to a particle size of 2-3 mm, and then flattened to a thickness of 0.15-0.20 mm and extracted with ethyl alcohol at 50-55 ° C for 8-9 hours with stirring. In a second step, the temperature is lowered to 25-30 ° C and methylene chloride is introduced. The extraction process is continued for 30-60 minutes, then the temperature is reduced to 18-20 ° C and the micelle is separated by filtration from the remainder of the plant material. The extractant is used for subsequent extraction. 1 s.p. crystals, 4 tab. ate with

Description

The invention relates to essential oil production and relates to the extraction of extractives from plant materials.

The purpose of the invention is to increase the yield of extractives.

To achieve this goal, the extraction is carried out with environmentally friendly volatile solvents - ethanol and methylene chloride.

Ethyl alcohol as an extractant is characterized by selective activity to the native water-alcohol-soluble components of biologically active plant materials. In addition, alcohol has the property of easily penetrating into the cell, contributing to the faster and more complete dissolution of extractable substances, desorbing substances from the cell walls and insoluble plant material. The presence of alcohol increases the rate of extraction and the dissolution of biologically active substances (BAS) in the extractant.

Methylene chloride belongs to the group of solvents with a high solubility. Almost all groups of biologically active substances in plant raw materials are dissolved in methylene chloride - saponins, chlorophyll, alkoloids, and volatile products. many vitamins, essential oils, tocopherols, flavonoids and their glycosides, etc.

In addition, methylene chloride dissolves well fatty biologically active substances - resins, fats, etc., which increases the biological value of the extract.

XI H)

about eating

00

Ј

Comparative extraction was carried out using liquefied carbon dioxide as an extractant, a mixture of freons 11 and 113 in a ratio of 90:10 and the proposed extractant,%:

Ethyl alcohol 40-60

Methylene Chloride: 60-40 (Table 1.3)

As plant raw materials, kbp, enz calamus, and thousands of shrubbery grass are used. Raw material Ш is crushed to a particle size of 2-3 mm, followed by flattening on smooth rollers to a thickness of 0.15-0.20 mm (Table 2).

The proposed extractant is used for 2-stage extraction.

The plant material is extracted with alcohol at 50-55 ° C for 8-9 hours with stirring at 60-80 rpm (Table 4). With stirring, the temperature is reduced to 25-30 ° C. Upon reaching the indicated temperature, the calculated amount of methylene chloride is introduced. Extraction is continued at 25-30 ° C, with stirring at a speed of 60-80 rpm for up to 30 minutes depending on the plant material.

The resulting mixture was cooled to 18-20 ° C, the miscella was separated and the extract was isolated from it in a known manner.

The invention is illustrated by the following examples.

Example 1. Extracted calamus root with a content of extractive substances of 6.2%, thousand herb grass with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 5-10 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%:

Ethyl alcohol50

Methylene Chloride50

Extraction of 2 steps over 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride at 25 ° C for 30 minutes.

The entire extraction process takes place with stirring at a speed of 60 rpm.

The yield of extractives and calamus root 5.2%.

The yield of extractive substances from the grass of thistle was 2.1%.

Example 2. Extract the root of calamus with a content of extractive substances of 6.2%, the grass of thousand tharwick with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%:

Ethyl alcohol 50 Methylene chloride 50 Extraction of 2-steps for 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The entire extraction process takes place with stirring at a speed of 60 rpm.

The yield of extractives from calamus root is 5.7%.

The yield of extractive substances from the grass of thousand capelin is 2.4%.

Example 3. Extract the calamus root with the content of extractive substances of 6.2%, the grass from the celery with the content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, then flattened into petals with a thickness of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%: Ethyl alcohol 50 Methylene chloride 50 Extraction 2-steps for 8 hours. 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The entire extraction process takes place with stirring at a speed of 60 rpm.

The yield of extractives from calamus root is 5.9%.

The yield of extractive substances from the grass of thousand capelin is 2.5%.

Example 4. Extract the calamus root with a content of extractive substances of 6.2%, the grass of a thousand capelin tree with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 6. In the extractant, the ratio of solvents,%:

Ethyl alcohol 50 Methylene chloride 50 Extraction of 2-steps for 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The entire extraction process takes place with stirring at a speed of 60 rpm. The yield of extractives from calamus root 5.5%. The yield of extractive substances from the grass of thousand capelin is 2.3%.

Example 5. Extracted calamus root with a content of extractive substances of 6.2%, thousand herb grass with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1:10. In the extractant, the ratio of solvents,%: Ethyl alcohol 50 Methylene chloride 50 Extraction 2-steps for 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 minutes at 25 ° C. The entire extraction process is carried out with stirring at a speed of 60 rpm.

The yield of extractives from calamus root is 5.9%. Extractive substances yield from grass

thousand capelis 2.5%. Example 6. Extract the calamus root with a content of extractive substances of 6.2%, the grass of a thousand cephyrus with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%: Ethyl alcohol 60 Methylene chloride 40 Extraction 2-steps for 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The entire extraction process takes place with stirring at a speed of 60 rpm. The yield of extractives from calamus root is 5.6%. The yield of extractive substances and herbs thousand of chistaris 2.3%. Example 7. Extract the calamus root with a content of extractive substances of 6.2%, the herb thousand of yarrow with a content of extractives of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%:

Ethyl alcohol 30 Methylene chloride 70

Extraction of 2 steps over 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The entire extraction process takes place with stirring at a speed of 60 rpm.

The yield of extractives from calamus root is 5.8%. The yield of extractive substances from the grass of thousand capelin is 2.4%. Example 8. Extract the root of calamus with the content of extractive substances of 6.2%, the grass of thousands of celery with the content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. Extragent solvent ratio,%:

Ethyl alcohol 50 Methylene chloride 50 Extraction of 2-steps over 7 hours 15 minutes. The first step is extraction with ethyl alcohol for 7 hours at 50 ° C. The second stage is extraction with methylene chloride for 15 min at 25 ° C. The whole process takes place with stirring at a speed of 60 rpm.

The yield of extractives from calamus root is 5.4%. The yield of extractive substances from the grass of thousand capelin is 2.2%. PRI me R 9. Extract the root of calamus with a content of extractive substances of 6.2%, the grass thousand of yarrow with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%:

Ethyl alcohol 50 Methylene chloride 50 Extraction of 2-steps over 9 hours 30 minutes. The first step is extraction with ethyl alcohol for 9 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The whole process takes place with stirring at a speed of 60 rpm. The yield of extractives from calamus root is 5.9%.

The yield of extractives from calamus root

The output of extractives from the grass

Example 10. Extracted calamus root with a content of extractive substances of 6.2%, thousands of herb of a stem tree with a content of extractive substances of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of plant materials: extractant 1: 8. In the extractant, the ratio of solvents,%: Ethyl alcohol 50 Methylene chloride 50 Extraction 2-steps for 8 hours 30 minutes. The first step is extraction with ethyl alcohol for 8 hours at 40 ° C. The second stage is extraction with methylene chloride for 30 min at 20 ° C. The whole process takes place with stirring at a speed of 60 rpm. The yield of extractives from calamus root 5.5%.

0

5

0

5

The yield of extractive substances from the grass of thousand capelin is 2.3%. Example 11. Extract the calamus root with a content of extractive substances of 6.2%, thousands of herb of a cephalopod with a content of extractives of 2.8%. Plant materials are crushed to a particle size of 2-3 mm, followed by flattening to a thickness of the petals of 0.15-0.20 mm. The ratio of vegetable raw materials: extractant 1: 8. In the extractant, the ratio of solvents,%:

Ethyl alcohol 50 Methylene chloride 50 Extraction of 2-steps for 8 hours 30 minutes, First step - extraction with ethyl alcohol for 8 hours at 50 ° C. The second stage is extraction with methylene chloride for 30 min at 25 ° C. The whole process takes place with stirring at a speed of 50 rpm. The yield of extractives from calamus root is 5.8%. The yield of extractive substances from the grass of thousand capelin is 2.4%.

Claims (2)

SUMMARY OF THE INVENTION 1. A method of obtaining an extract from an essential oil plant material, including grinding, extraction, filtering the obtained miscella and distilling off the solvent, characterized in that, in order to increase the yield of extractives, grinding is carried out to a particle size of 2-3 mm, and then subjected to conditioning to a thickness of the lobe 0.15-0.20 mm, extraction is carried out in two stages, in the first of which ethanol is used as an extractant and the process is carried out at 50-55 ° C for 8-9 hours, and in the second, methylene chloride is used, and the process is carried out at 25-30 ° C for 30-60 minutes, moreover, the ratio of feed: extractant is 1: 8. 2. The method according to claim 1, characterized in that the ratio of ethanol: methylene chloride is (40-60): (60-40), TABLE 1 Comparative extraction results with various extractants Comparative extraction results depending on the degree of grinding of raw materials Table3 Comparative extraction results depending on the ratio of plant material to extractant Table 2 Table 4 Comparative extraction results versus time factor Extract extract calamus root containing 6.2% of extractive substances I stage - 7 h; II stage -15 min I stage - 8 h; II stage - 30 min I stage - 9 h; II stage - 45 min I stage - 10 hours II stage - 1 h The output of extractive substances,%, from herbs thousand capelin containing 2.8% of extractive substances 5,4 2.2 5.9 2,5 5.9 2,5 5.9 2,5