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Extraction and separation method of alkaloid in traditional Chinese medicinal material

A separation method and alkaloid technology, applied in the direction of material separation, analysis materials, measurement devices, etc., can solve the problems of low separation efficiency, cumbersome operation, poor versatility, etc., and achieve the goal of optimizing analysis methods, improving analysis efficiency, and high accuracy Effect

Active Publication Date: 2014-12-03
北京泰克美高新技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the above methods generally have the disadvantages of cumbersome operation, low separation efficiency, and poor versatility. The current chromatographic separation methods generally ignore the alkaloids in the strong polar part.

Method used

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  • Extraction and separation method of alkaloid in traditional Chinese medicinal material
  • Extraction and separation method of alkaloid in traditional Chinese medicinal material
  • Extraction and separation method of alkaloid in traditional Chinese medicinal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Extraction: take the dry bark of Jujube sylvestris, crush it, weigh 10g, add 10 times the weight of ethanol with a mass concentration of 60% (adjust the pH to 2.5 with acetic acid) for reflux extraction for 1 hour, filter; collect the filter residue, and then Use 10 times the weight of ethanol with a mass concentration of 60% (adjust the pH to 2.5 with acetic acid) for reflux extraction for 1 hour, filter, and combine the two filtrates to a total of 185 mL. The extract was concentrated to 10 mL under reduced pressure to obtain sample 1, which was reserved for testing.

[0058] 2. HPLC analysis

[0059] Chromatographic conditions:

[0060] Condition ①——Chromatographic column: TechMate C18-ST (150mm×4.6mm, 5μm); mobile phase: acetonitrile:water=30:70, adjust the pH to 2.5 with formic acid; flow rate: 1.0mL / min, column temperature: 40°C.

[0061] Condition ②——Chromatographic column: TechMate CR(1:5)-ST (150mm×2.0mm, 5μm); mobile phase A: acetonitrile: water = 30:70, f...

Embodiment 2

[0068] 1. Extraction: Take the dried Jujube fruit, crush it, weigh 10g, add 10 times the weight of ethanol with a mass concentration of 60% (use acetic acid to adjust the pH to 3.5) and reflux for extraction for 1 hour, filter; collect the filter residue, and then use weight 10 times the volume and mass concentration of 60% ethanol (adjust the pH to 3.5 with acetic acid) for reflux extraction for 1 hour, filter, and combine the two filtrates to a total of 180 mL. The extract was concentrated to 10 mL under reduced pressure to obtain sample 2, which was reserved for testing.

[0069] 2. HPLC analysis

[0070] Chromatographic conditions:

[0071] Condition ①——Chromatographic column: TechMate C18-ST (150mm×4.6mm, 5μm); mobile phase: acetonitrile:water=30:70, adjust the pH to 3.5 with formic acid; flow rate: 1.0mL / min, column temperature: 40°C.

[0072] Condition ②——Column: TechMate CR(1:5)-ST (150mm×2.0mm, 5μm); mobile phase A: acetonitrile: water = 30:70, formic acid to adjust...

Embodiment 3

[0079] 1. Extraction: take the dry golden jujube bark, crush it, weigh 10g, add 10 times the weight and 60% ethanol (adjust the pH to 2.0 with acetic acid) for reflux extraction for 1 hour, filter; collect the filter residue, and use The weight is 10 times the amount and the mass concentration is 60% ethanol (adjust the pH to 2.0 with acetic acid) for reflux extraction for 1 hour, filter, and combine the two filtrates, a total of 190mL. The extract was concentrated to 10 mL under reduced pressure to obtain sample 3, which was reserved for testing.

[0080] 2. HPLC analysis

[0081] Chromatographic conditions:

[0082] Condition ①——Chromatographic column: TechMate C18-ST (150mm×4.6mm, 5μm); mobile phase: acetonitrile:water=30:70, adjust the pH to 2.0 with formic acid; flow rate: 1.0mL / min, column temperature: 40°C.

[0083] Condition ②——Column: TechMate CR(1:5)-ST (150mm×2.0mm, 5μm); mobile phase A: acetonitrile: water = 30:70, formic acid to adjust the pH value to 2.0; mobil...

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Abstract

The invention relates to an extraction and separation method of an alkaloid in a traditional Chinese medicinal material. The method comprises the following steps: 1) extracting the traditional Chinese medicinal material by using an alcohol solvent, thereby obtaining a traditional Chinese medicinal extract; 2) bonding the traditional Chinese medicinal extract with a porous silica gel column through an octadecyl and collecting a solution flows within the first five minutes; and 3) bonding the solution obtained in the step 2) with a chromatographic column of a mixed filling material of C18 and cation exchange groups, and performing a gradient elution on the chromatographic column, thereby obtaining a separated alkaloid. As the method is used, the analysis efficiency is improved greatly; the analysis result is high in accuracy; the experimental period is shortened because the process is operated simply and easily; the high universality is realized, i.e., the alkaloid in a part with strong polarity is not ignored; the extraction is performed accurately; and the alkaloid in an extracting solution is separated, so that the possibility of discovering a new alkaloid and especially the alkaloid with the strong polarity is enlarged greatly.

Description

technical field [0001] The invention relates to the field of extraction and separation of traditional Chinese medicines, in particular to a method for extraction and separation of alkaloids in Chinese medicinal materials. Background technique [0002] Alkaloids are nitrogen-containing basic organic compounds in plants, and most of them have obvious physiological activities, so they are often the active ingredients of many Chinese herbal medicines. Most of the alkaloids come from the plant kingdom, and they are mostly distributed in plants of Papaveraceae, Fabaceae, Fangjiaceae, Ranunculaceae and other families. The content of alkaloids is generally low, mostly less than 1%, and the content of vincristine in periwinkle is only one millionth. A plant often contains several or dozens of alkaloids. Therefore, the extracted total alkaloids need to be further separated to remove impurities and interferers to ensure the accuracy of the analysis results. [0003] At present, in o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 王兵陈尚义谭鹏邢艳平戴学良王涛林蔚梅王彦鹏
Owner 北京泰克美高新技术有限公司