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Method for extracting scopolamine by virtue of membrane separation technique

A scopolamine and membrane separation technology, applied in the direction of organic chemistry, can solve the problems of difficult to meet high-purity product purity, tedious and time-consuming extraction process, low scopolamine content, etc., to achieve shortened production time, low production cost, and high product yield. rate effect

Inactive Publication Date: 2017-10-10
ANHUI DEXINJIA BIOPHARM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction of scopolamine mainly uses Dajinhua as raw material, and generally uses organic solvents such as chloroform to extract or directly perform column chromatography separation after crude extraction. The organic solvent extraction process is cumbersome and time-consuming with serious organic pollution, and the purity of the final product is also difficult. To meet the high-purity requirements, and repeated extractions are likely to cause loss of raw materials, and the yield is low. However, the method of directly performing column chromatography separation after crude extraction is extremely low in the content of scopolamine in the crude extract, and it is necessary to obtain a certain amount of high-purity substances. A large amount of raw material liquid is purified by column, the efficiency is extremely low, and the application in industrial production will seriously slow down the production progress. Therefore, inventing a preparation method of scopolamine with high product purity and high production efficiency has very broad market prospects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The method that present embodiment adopts membrane separation technology to extract scopolamine is as follows:

[0037] 1. Pretreatment

[0038] Put the raw material Dajinhua in a vacuum drying oven at 40°C for 24 hours, take it out, crush it with a pulverizer and pass it through a 100-mesh sieve to obtain Dajinhua powder;

[0039] 2. Separation and extraction

[0040] According to the ratio of mass volume ratio 1g: 9mL, add HCl solution with a mass concentration of 0.1% to the datura powder, mix it and then ultrasonically treat it for 30min, the ultrasonic power is 250W, and the frequency is 40Hz, and the material after ultrasonic treatment is suction-filtered to obtain the filter residue and For the filtrate, add HCl solution again to the obtained filter residue to repeat the above-mentioned ultrasonic treatment process, and merge the filtrate obtained twice after suction filtration, which is the scopolamine extract;

[0041] 3. Ultrafiltration to remove impurities ...

Embodiment 2

[0056]The preparation process of this example is the same as that of Example 1, except that the membrane molecular weight cut-off in the ultrafiltration impurity removal process in step 3 is 6K.

[0057] Take a certain amount of scopolamine extract and place it in a rotary evaporator to recover the solid to obtain a dry extract, weigh it, then take an equal amount of the effluent after ultrafiltration to remove impurities, put it in a rotary evaporator to recover the solid to obtain a dry extract, and calculate the weight according to the formula Calculate the impurity removal rate, the impurity removal rate=(the dry solid of the equivalent scopolamine extract solution-the dry solid of the equivalent scopolamine ultrafiltration dialysate) / the dry solid × 100% of the equivalent scopolamine extract solution, get the impurity removal of this embodiment The rate is 96.17%.

[0058] Get the scopolamine extract and inject it into a high-performance liquid chromatograph for detection...

Embodiment 3

[0060] The preparation process of this example is the same as that of Example 1, except that the membrane molecular weight cut-off in the ultrafiltration impurity removal process in step 3 is 50K.

[0061] Take a certain amount of scopolamine extract and place it in a rotary evaporator to recover the solid to obtain a dry extract, weigh it, then take an equal amount of the effluent after ultrafiltration to remove impurities, put it in a rotary evaporator to recover the solid to obtain a dry extract, and calculate the weight according to the formula Calculate the impurity removal rate, the impurity removal rate=(the dry solid of the equivalent scopolamine extract solution-the dry solid of the equivalent scopolamine ultrafiltration dialysate) / the dry solid × 100% of the equivalent scopolamine extract solution, get the impurity removal of this embodiment The rate is 80.74%.

[0062] Get the scopolamine extract and inject it into a high-performance liquid chromatograph for detecti...

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Abstract

The invention discloses a method for extracting scopolamine by virtue of a membrane separation technique. A scopolamine finished product is prepared by the following steps: raw material pretreatment, preparation of a scopolamine extracting solution, ultrafiltration impurity removal, sodium filter desalination, reduced pressure concentration and drying, resin bed purification, scopolamine salt formation and the like. The scopolamine extracting solution is preliminarily purified and concentrated through operations of impurity removal, desalination and the like by virtue of the membrane separation technique and is highly purified through column chromatography, so that the production time is greatly shortened, and the production efficiency is improved; and compared with a conventional method, the product yield and the product purity are relatively high, and the method is applicable to industrial production.

Description

technical field [0001] The invention relates to a method for extracting scopolamine by adopting membrane separation technology, which belongs to the field of separation and purification of medicines. Background technique [0002] Scopolamine is an alkaloid with the strongest pharmacological action in belladonna. It is a viscous syrupy liquid at room temperature with a bitter and pungent taste; it is easily soluble in ethanol, chloroform, acetone and hot water, and slightly soluble in benzene and petroleum ether. It can form crystalline salts with a variety of inorganic or organic acids. The effect of scopolamine is similar to that of atropine. Its mydriasis and inhibition of glandular secretion are stronger than atropine. It has an exciting effect on the respiratory center, but it has a significant inhibitory effect on the cerebral cortex. It also has the effects of dilating capillaries, improving microcirculation, and anti-seasickness. It is clinically used as a sedative, ...

Claims

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Application Information

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IPC IPC(8): C07D451/10
CPCC07D451/10
Inventor 许坤张文成付传香惠爱玲
Owner ANHUI DEXINJIA BIOPHARM
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