Detection method of plant extract or preparation

A plant extract and detection method technology, applied in the field of detection of plant extracts or their preparations, can solve the problems of restricting preparation production monitoring and content determination, increasing column temperature, failing to improve separation effect, etc. The effect of improved separation and protection

Pending Publication Date: 2020-04-28
GUANGXI WEHAND BIO PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will greatly limit the production monitoring and assay of related preparations
[0007] At the same time, the study found that traditional methods such as adjusting the mobile phase ratio, changing the pH value of the mobile phase, and increasing the column temperature cannot improve the separation effect.

Method used

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  • Detection method of plant extract or preparation
  • Detection method of plant extract or preparation
  • Detection method of plant extract or preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Select alkaloid standard substances with similar structures, 1-deoxynojirimycin (1-DNJ) (1), buckwheat (Fagomine) (2) and 1,4-dideoxy-1,4- Amino-D-arabinitol (1,4-dideoxy-1,4-imino-D-arabinitol, DAB) (3), the structural formula is as follows:

[0035]

[0036]

[0037] Weigh an appropriate amount of reference substance, add water to dissolve, dilute and prepare an alkaloid reference solution containing 0.02 mg of 1-DNJ, 0.02 mg of buckwheatine, and 0.02 mg of DAB in each 1 ml and 0.1 mg of 1-DNJ, buckwheatine, and Each DAB is 0.02 mg mixed alkaloid reference substance solution.

[0038] Accurately measure 1ml each of 1-DNJ reference solution, DAB reference solution, buckwheat alkali reference solution and the above-mentioned mixed alkaloid reference solution, and use the following detection methods for detection:

[0039] Detection steps: Put in a stoppered test tube, add 200mmol / L sodium bicarbonate solution, shake well, then precisely add 2ml5mmol / L fluorenylme...

Embodiment 2

[0048] Take 100 g of Sangteyou No. 2 mulberry branches, add water, heat and reflux for extraction, filter to remove impurities, separate the cation resin and anion resin, concentrate and dry to obtain the mulberry branch extract.

[0049] Take about 100mg of mulberry branch extract, weigh it accurately, put it in a 50ml measuring bottle, add 40ml of water, ultrasonically dissolve it for 20min, let it cool to room temperature, add water to dilute to the mark, shake well, filter, and accurately measure 1ml of the subsequent filtrate, set In a 10ml measuring bottle, add water to dilute to the mark, shake well to obtain the test solution; accurately measure 1ml of the test solution, put it in a stoppered test tube, add 1ml of 200mmol / L sodium bicarbonate solution precisely, shake well, and then Accurately add 1ml of 5mmol / L fluorenylmethyl-9-chloroformate (FMOC-Cl) acetone solution, shake well, heat at 30°C for 30min, accurately add 4ml of 0.1% acetic acid, shake well, filter, accu...

Embodiment 3

[0054] Take about 100 mg of the mulberry branch extract prepared in Example 2, weigh it accurately, put it in a 50 ml measuring bottle, add 40 ml of water, dissolve it by ultrasonication for 20 minutes, let it cool to room temperature, add water to dilute to the scale, shake well, filter, and accurately measure Add 1ml of the filtrate, put it in a 10ml measuring bottle, add water to dilute to the mark, and shake well to obtain the test solution; accurately measure 1ml of the test solution, put it in a stoppered test tube, and precisely add 1ml of 200mmol / L sodium bicarbonate solution , shake well, then precisely add 1ml of 5mmol / L 9-fluorenylmethyl chloroformate (FMOC-Cl) acetone solution, shake well, heat at 30°C for 30min, precisely add 4ml of 0.1% acetic acid, shake well, filter, and precisely absorb 10 μl of the filtrate was injected into the liquid chromatograph.

[0055] Chromatographic column and elution conditions: use octadecylsilane bonded silica gel as filler, aceto...

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Abstract

The invention relates to a method for detecting alkaloid in a plant extract or a preparation. The alkaloid optionally comprises one or more of fagopyrin and 1, 4-dideoxy-1, 4-imino group -D-arabitol.The method comprises the following steps: carrying out a derivatization reaction on a to-be-detected plant extract or the preparation by using a derivatization reagent to obtain a derivatization product containing an alkaloid derivative; and (2) carrying out chromatographic analysis on the derivatization product obtained in the step (1), wherein the temperature of a chromatographic column is 5+/-2-20+/-2 DEG C. According to the method, multiple alkaloid components with similar structures can be detected at the same time, and production monitoring and content determination of the related preparations are facilitated.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a detection method of a plant extract or a preparation thereof. Background technique [0002] Alkaloids are a class of nitrogen-containing basic organic compounds that exist in nature (mainly in plants, but also in a small number of animals). There are more than 100 families of plants containing alkaloids, and the same plant often contains several There are several or even dozens of alkaloids. For example, mulberry contains at least 4 alkaloids, ephedra contains 7 alkaloids, and periwinkle contains more than 60 alkaloids. Studies have found that alkaloids have many pharmacological activities, such as lowering blood sugar, lowering blood pressure, anti-tumor, anti-inflammatory and analgesic, antibacterial and anti-viral, etc., which are widely used in clinical treatment of various diseases, but at the same time, research has also found that some alkaloids are harmfu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/30G01N30/34G01N30/74G01N2030/067
Inventor 刘玉玲夏学军申琪琪刘志华金毅群朱向阳汪仁芸邹媛媛
Owner GUANGXI WEHAND BIO PHARMA CO LTD
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