CN105726837A - Method for extracting effective components of pinelliae rhizoma praeparatumcum zingibere et alumina through ultrasonic-assisted solvent method - Google Patents
Method for extracting effective components of pinelliae rhizoma praeparatumcum zingibere et alumina through ultrasonic-assisted solvent method Download PDFInfo
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- CN105726837A CN105726837A CN201410756296.XA CN201410756296A CN105726837A CN 105726837 A CN105726837 A CN 105726837A CN 201410756296 A CN201410756296 A CN 201410756296A CN 105726837 A CN105726837 A CN 105726837A
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Abstract
The invention discloses a method for extracting effective components of pinelliae rhizoma praeparatumcum zingibere et alumina through an ultrasonic-assisted solvent method. The method is characterized by comprising the following steps: (1) pre-treatment of medicinal materials; (2) ultrasonic extraction; (3) preparation of an aqueous acid solution; (4) extraction; and (5) crystallization. According to the method, a nontoxic aqueous acid solution is taken as an extracting agent; the extraction time is short; and the produced product is safe. Cells of the medicinal materials are broken through stirring and a high-speed intense cavitation effect generated through ultrasonic wave, thereby simplifying operation processes and improving extraction efficiency. The method is green, eco-friendly, efficient, and energy-saving.
Description
Technical field
The invention belongs to ultrasonic assistant extract by solvents technical field, be specifically related to a kind of method that ultrasonic-assistant solvent method extracts Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient.
Background technology
Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens), refers to that Rhizoma Pinelliae fresh ginger or fresh ginger, Alumen boil dry Preparation process product altogether dry.According to 2010 version " Chinese Pharmacopoeia " record, Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) is pungent, warm, returns spleen, stomach, lung meridian, and function warming middle-JIAO reduces phlegm, stopping nausea and vomiting by lowering the adverse flow of QI, for vomiting due to fluid-retention, gastral cavilty feeling of fullness.Its method for making is: take the clean Rhizoma Pinelliae, size separately, be soaked in water to interior without the dry heart time, take out；Separately take Rhizoma Zingiberis Recens section and decoct soup, add Alumen well-done altogether with the Rhizoma Pinelliae, take out, dry or dry in the air to half-dried, dry；Or shave, dry.Poor operability in actual production process, product quality is difficult to control to, and the effective ingredient of the Rhizoma Pinelliae easily runs off in immersion process, and it is also poor with the effect of Alumen that the Rhizoma Pinelliae absorbs Rhizoma Zingiberis Recens, reduces the drug effect of Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) product all to some extent.The traditional extraction process of current Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient also exists the shortcomings such as yield is low, loss is bigger, and product exists dissolvent residual, poor stability；Operating process is relatively complicated, time-consuming, cost is high and extraction efficiency is relatively low.
Summary of the invention
For prior art exists Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient extraction yield is low, lose bigger, consume energy higher problem, in order to improve the extraction ratio of Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient, there is provided that a kind of extraction ratio is high, save solvent, the process of extraction time is short, less costly and applicable industrialization continuity produces ultrasonic assistant extract by solvents Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient, the extraction process of Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) is easily operated, the constant product quality obtained.
The technical scheme that the present invention takes is:
A kind of ultrasonic-assistant solvent method extracts the method for Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient, it is characterised in that specifically include following steps:
(1) medical material pretreatment: pulverized by Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) tuber, crosses 90 mesh sieves, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder；
(2) supersound extraction: be that 1:25mL soaks 24 hours by mass volume ratio by ethanol that Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder and volume fraction are 95%, at power 180-220W, when temperature 50 C, supersound extraction 60 minutes；Control vacuum 0.07～0.09MPa sucking filtration, obtain filtrate；
(3) acid liquid is prepared: step (2) gained filtrate is controlled vacuum is 0.07～0.09MPa, and temperature is 60-65 DEG C and is evaporated to without ethanol, is cooled to room temperature；Adding hydrochloric acid, dissolve, making density is 1.00～1.30, stands, and filters, obtains acid liquid；
(4) extract: by step 3) gained acid liquid petroleum ether extraction, the raffinate strong aqua ammonia obtained regulates pH to 8-9 and obtains alkaline solution；Being extracted with ethyl acetate, it is 0.07～0.09MPa that the extract obtained controls vacuum, and temperature is 45-55 DEG C and is evaporated to without ethyl acetate, is cooled to room temperature and obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract；
(5) crystallization: by step (4) gained Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract anhydrous alcohol solution, stands, crystallization, filters, with the absolute ethanol washing crystallization of pre-cooling, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens).
In described step (4), acid liquid and petroleum ether volume ratio are 1: 1～3；The volume ratio of described alkaline solution and ethyl acetate is 1: 1～3.
The invention have the benefit that
(1) present invention adopts nontoxic acid liquid as extractant, and extraction time is short, makes the product prepared have safety.
(2) utilize high speed, strong cavitation effect and the stirring action that ultrasound wave produces to destroy the cell of medical material, simplify operating process, improve extraction efficiency, there is green, environmental protection, efficient, energy-conservation advantage.
Detailed description of the invention
A kind of ultrasonic-assistant solvent method extracts the method for Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient, it is characterised in that specifically include following steps:
(1) medical material pretreatment: pulverized by Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) tuber, crosses 90 mesh sieves, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder；
(2) supersound extraction: be that 1:25mL soaks 24 hours by mass volume ratio by ethanol that Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder and volume fraction are 95%, at power 180-220W, when temperature 50 C, supersound extraction 60 minutes；Control vacuum 0.07～0.09MPa sucking filtration, obtain filtrate；
(3) acid liquid is prepared: step (2) gained filtrate is controlled vacuum is 0.07～0.09MPa, and temperature is 60-65 DEG C and is evaporated to without ethanol, is cooled to room temperature；Adding hydrochloric acid, dissolve, making density is 1.00～1.30, stands, and filters, obtains acid liquid；
(4) extract: by step 3) gained acid liquid petroleum ether extraction, the raffinate strong aqua ammonia obtained regulates pH to 8-9 and obtains alkaline solution；Being extracted with ethyl acetate, it is 0.07～0.09MPa that the extract obtained controls vacuum, and temperature is 45-55 DEG C and is evaporated to without ethyl acetate, is cooled to room temperature and obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract；
(5) crystallization: by step (4) gained Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract anhydrous alcohol solution, stands, crystallization, filters, with the absolute ethanol washing crystallization of pre-cooling, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens).
In described step (4), acid liquid and petroleum ether volume ratio are 1: 1～3；The volume ratio of described alkaline solution and ethyl acetate is 1: 1～3.
Claims (2)
1. the method that a ultrasonic-assistant solvent method extracts Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient, it is characterised in that specifically include following steps:
(1) medical material pretreatment: pulverized by Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) tuber, crosses 90 mesh sieves, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder；
(2) supersound extraction: be that 1:25mL soaks 24 hours by mass volume ratio by ethanol that Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) medicated powder and volume fraction are 95%, at power 180-220W, when temperature 50 C, supersound extraction 60 minutes；Control vacuum 0.07～0.09MPa sucking filtration, obtain filtrate；
(3) acid liquid is prepared: step (2) gained filtrate is controlled vacuum is 0.07～0.09MPa, and temperature is 60-65 DEG C and is evaporated to without ethanol, is cooled to room temperature；Adding hydrochloric acid, dissolve, making density is 1.00～1.30, stands, and filters, obtains acid liquid；
(4) extract: by step 3) gained acid liquid petroleum ether extraction, the raffinate strong aqua ammonia obtained regulates pH to 8-9 and obtains alkaline solution；Being extracted with ethyl acetate, it is 0.07～0.09MPa that the extract obtained controls vacuum, and temperature is 45-55 DEG C and is evaporated to without ethyl acetate, is cooled to room temperature and obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract；
(5) crystallization: by step (4) gained Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) extract anhydrous alcohol solution, stands, crystallization, filters, with the absolute ethanol washing crystallization of pre-cooling, obtains Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens).
2. the method that ultrasonic-assistant solvent method extracts Rhizoma Pinelliae (processed with Rhizoma Zingiberis Recens) effective ingredient according to claim 1, it is characterised in that in described step (4), acid liquid and petroleum ether volume ratio are 1: 1～3；The volume ratio of described alkaline solution and ethyl acetate is 1: 1～3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410756296.XA CN105726837A (en) | 2014-12-11 | 2014-12-11 | Method for extracting effective components of pinelliae rhizoma praeparatumcum zingibere et alumina through ultrasonic-assisted solvent method |
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| CN201410756296.XA CN105726837A (en) | 2014-12-11 | 2014-12-11 | Method for extracting effective components of pinelliae rhizoma praeparatumcum zingibere et alumina through ultrasonic-assisted solvent method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
| CN109125535A (en) * | 2018-05-11 | 2019-01-04 | 重庆医科大学 | A kind of method of Pinellia Ternate surface devulcanization |
-
2014
- 2014-12-11 CN CN201410756296.XA patent/CN105726837A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109125535A (en) * | 2018-05-11 | 2019-01-04 | 重庆医科大学 | A kind of method of Pinellia Ternate surface devulcanization |
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
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Application publication date: 20160706 |
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