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Recycling method of extracting solvent of galangal dropping pill extract

A technology for extracting solvents and attaching dripping pills, which is applied in the field of reuse of extracting solvents of Liangfu dripping pills, can solve the problems of reduced transfer rate of galangin, lower yield of extracts, and inability to recycle ethyl acetate, etc. Achieve the effects of reducing storage difficulty, guaranteeing yield, and reducing production costs

Pending Publication Date: 2022-08-02
贵州黄果树立爽药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] This application provides a method for reusing the extraction solvent of the Liangfu dropping pill extract, which is used to solve the problem in the prior art that the ethyl acetate solvent obtained by extracting and recovering the Liangfu dropping pill extract can be reused in the Liangfu dropping pill When the extract is extracted, the yield of the extract is reduced, and the transfer rate of the main active ingredient galangin in the extract is reduced, resulting in a technical problem that a large amount of recovered ethyl acetate cannot be recycled.

Method used

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  • Recycling method of extracting solvent of galangal dropping pill extract
  • Recycling method of extracting solvent of galangal dropping pill extract
  • Recycling method of extracting solvent of galangal dropping pill extract

Examples

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Effect test

Embodiment 1~5

[0049] Proceed as follows:

[0050] 1) The ethyl acetate solvent obtained by distillation under reduced pressure is distilled and dried, and the steamed gas passes through Na 2 CO 3 solution to obtain a recovery solution;

[0051]2) The recovered solution obtained in step 1) is distilled under normal pressure, and the obtained fraction is collected at 77°C;

[0052] 3) adding a desiccant to the obtained fraction in a ratio of 1 g:100 mL, and filtering with a 0.45 m microporous membrane after shaking overnight to obtain a filtrate;

[0053] 4) measure the moisture content in the gained filtrate, repeat steps 2) to 3) when moisture content>5% until the moisture content in the gained filtrate is less than or equal to 5% and stop to obtain ethyl acetate for reuse;

[0054] 5) Mix the recycled ethyl acetate with the unused ethyl acetate solvent in a volume ratio of 3:1 to obtain a recycled ethyl acetate solvent.

[0055] The method reagents and moisture content determination re...

Embodiment 6

[0059] Embodiment 6 measures the refractive index of the obtained solvent

[0060] Measured by the method under Item 0622 of Chinese Pharmacopoeia 2020 Edition, Part 4, and the obtained circulating ethyl acetate solvent after the above method was extracted in Example 1. The refractive index is about 1.372 (n=5), which is in line with the Chinese Pharmacopoeia. The refractive index of ethyl acetate solvent is specified.

[0061] In the remaining examples, the obtained circulating ethyl acetate test results are similar to the results obtained in Example 1, and are not described here.

Embodiment 7

[0062] Example 7 Gas Chromatography Determination

[0063] Adopt the gas chromatography method under Item 0521 of 4 General Rules of Chinese Pharmacopoeia in 2020, to measure the obtained circulating ethyl acetate solvent in Example 1, and the obtained results are as follows figure 2 shown.

[0064] Depend on figure 2 The result shows that the relevant impurities in the obtained circulating ethyl acetate slightly increase. According to the peak area normalization method, the sum of the peak areas of each impurity is about 0.2% of the main peak area, which meets the limit requirement.

[0065] In the remaining examples, the obtained circulating ethyl acetate test results are similar to the results obtained in Example 1, and are not described here.

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Abstract

The invention discloses a reutilization method of a galangal dropping pill extract extraction solvent, which comprises the following steps: 1) distilling and drying an ethyl acetate solvent obtained by reduced pressure distillation, and enabling the evaporated gas to pass through a Na2CO3 solution to obtain a recovery solution; 2) carrying out atmospheric distillation on the recovered solution obtained in the step 1), and collecting the obtained fraction at 77 DEG C; 3) adding a drying agent into the obtained fraction according to a ratio of 1g: 100mL, oscillating overnight, and filtering by using a 0.45 m microporous filter membrane to obtain a filtrate; (4) measuring the moisture content in the obtained filtrate until the moisture content in the obtained filtrate is less than or equal to 5% to obtain recycled ethyl acetate; and 5) mixing the recycled ethyl acetate and the unused ethyl acetate solvent according to a volume ratio of 3: 1 to obtain the recycled ethyl acetate solvent. The recycling ethyl acetate obtained by the method is used for maintaining the extraction yield of the extract, and can replace a new ethyl acetate solvent, so that the amount of ethyl acetate waste liquid is reduced, and the storage difficulty and the production cost of enterprises are reduced.

Description

technical field [0001] The application relates to the technical field of production methods of traditional Chinese medicine preparations, in particular to a method for reusing the extraction solvent of Liangfu dropping pills extract. Background technique [0002] Liangfu Dropping Pill is composed of two traditional Chinese medicines, Galangal and Cyperus officinalis. Acid embolism. The existing Liangfu dropping pill extract extraction process is as follows: [0003] Take 93.75g each of galangal and Cyperus officinalis (vinegar) respectively, crush galangal into the coarsest powder, crush Cymbidium officinalis, add 8 times the amount of ethyl acetate, soak for 1 hour, and extract by reflux for 2 times, 1 hour each time, Filter, combine the filtrates, and recover the filtrate under reduced pressure to a clear paste without ethyl acetate smell (relative density at 60° C. is 1.07), that is, it is obtained. [0004] In the existing extraction process, ethyl acetate is used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/54C07C67/56C07C69/14
CPCC07C67/54C07C67/56C07C69/14
Inventor 蔡雪飞
Owner 贵州黄果树立爽药业有限公司