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Method for detecting picrasma quassioides alkali content in picrasma quassioides

A detection method, a technology of picrophylline, which is applied in the field of analytical chemistry and can solve problems such as quantification

Active Publication Date: 2013-12-04
GUANGZHOU BAIYUSN HUTCHISON WHAMPOA CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no quantitative determination item in the quality standard of bitterwood medicinal materials, and the standard needs to be improved urgently. The current quantitative analysis method for bitterwood in bitterwood cannot simultaneously quantify bitterwood B, bitterwood hexamate and bitterwood D

Method used

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  • Method for detecting picrasma quassioides alkali content in picrasma quassioides
  • Method for detecting picrasma quassioides alkali content in picrasma quassioides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0061] Embodiments 1-5 adopt different chromatographic conditions to detect picrophylline

[0062] Take appropriate amount of three kinds of standard products of bitternine B, bitternine and bitternine respectively, weigh them accurately, put them in a 50mL measuring bottle, add methanol to make each 1mL contain bitternine B 10μg, bitternine 30μg , a solution of 20 μg of matrine, as a standard solution. Store in the refrigerator at 4°C for later use.

[0063] After drying and pulverizing the bitter wood medicinal material, the coarse powder is about 1g, accurately weighed, placed in a stoppered Erlenmeyer flask, accurately added 50mL of 80% methanol, weighed, refluxed for 1.5h, let cool, and added 80% methanol to make up for the loss Weight, shake well, take the supernatant, filter with a microporous membrane (0.45μm), take the subsequent filtrate, as the solution to be tested.

[0064] Gradient elution program: 0min~35min, the volume fraction of phase A is from 5% to 45%; ...

Embodiment 6

[0074] Embodiment 6 The linear range investigation of the method provided by the present invention

[0075] Take appropriate amount of three kinds of standard products of bitternine B, bitternine and bitternine respectively, weigh them accurately, put them in a 50mL measuring bottle, add methanol to make each 1mL contain bitternine B 10μg, bitternine 30μg , a solution of 20 μg of matrine, as a standard solution. Store in the refrigerator at 4°C for later use.

[0076] Take 1 μL, 2 μL, 5 μL, 10 μL, 15 μL, and 30 μL of the standard solution respectively, and follow the method provided in Example 1 of the present invention to inject samples in sequence for determination. The standard curve was drawn with the measured peak area as the ordinate and the injection volume (μg) as the abscissa. The results are shown in Table 2

[0077] Table 2 Regression equation, correlation coefficient and linear range of bitternine B, bitternine and bitternine D

[0078] Compound name ...

Embodiment 7

[0079] Embodiment 7 The precision detection of the method provided by the present invention

[0080] Take about 1g of the coarse powder after drying and crushing the bitter wood medicinal material, accurately weigh it, put it in a stoppered Erlenmeyer flask, add 50mL of 80% methanol accurately, weigh it, reflux extraction for 1.5h, let it cool, add 80% methanol to make up for the loss Shake well, take the supernatant, filter it with a microporous membrane (0.45 μm), and take the subsequent filtrate as the solution to be tested.

[0081] Get the solution to be tested, according to the method provided in Example 1 of the present invention, continuously sample 6 times, each 10 μ L, record the peak area of ​​picerine B, picerine hexamate, picerine D, calculate the relative standard deviation, the result As shown in Table 3, the results show that adopting the method provided by the invention to continuously measure 6 times of detection of bitternine B, bitternine and bitternine D i...

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Abstract

The invention relates to the analytical chemistry field, particularly to a method for detecting picrasma quassioides alkali content in picrasma quassioides. The method comprises the following steps: preparing 1-carbomethoxy-Beta-carboline, nigakinone, and metiiylnigakinone standard solutions and drawing a standard curve; drying and smashing picrasma quassioides, and extracting to obtain a solution to be detected; detecting, wherein the detection chromatographic condition is that a C18 chromatographic column is adopted, the column temperature is 20-40 DEG C, the detection wave length is 205-280 nm, acetonitrile is taken as an A phase of a mobile phase while acid water is taken as a B phase of the mobile phase, the flow velocity is 1 mL / minute, and the elution procedures are performed in the way that the volume percent of acetonitrile is changed from 5% to 45% during the period from 0 minutes to 35 minutes, from 45% to 80 % during the period from 35 minutes to 40 minutes, from 80% to 90% during the period from 40 minutes to 50 minutes, and from 90% to 95% during the period from 50 minutes to 60 minutes; computing the content of three kinds of picrasma quassioides alkali as per the standard curve, wherein acids in acid water are phosphoric acid, formic acid or acetic acid, and the volume fraction of acid in acid water is 0.1-1%. The method can be used for the ration of three kinds of picrasma quassioides alkali at one time.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting the content of bitterwood in bitterwood. Background technique [0002] Bitterwood is the dry branches and leaves of Picrasma quassioides (D.Don) Benn. It is recorded in the 2010 edition of "Pharmacopoeia of the People's Republic of China". Cold in nature, bitter in the mouth. It has the effects of clearing heat, removing dampness and detoxifying; it is used to treat wind-heat cold, sore throat, diarrhea and dysentery, wet boils, poisonous snake bites, etc. It is the main raw material of Chinese patent medicines such as Xiaoyan Lidan Tablets. Bitterwood mainly contains alkaloids, bittersin, bitterwood lactone and so on. The alkaloids are mainly bitterwood, and the content of bitterwood B, bitterwood a and bitterwood D has an important influence on the quality of bitterwood medicinal materials. The structure of picrophylline (1-methoxyformyl-β-carbalin...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 姚小华林青李楚源黄琳匡艳辉
Owner GUANGZHOU BAIYUSN HUTCHISON WHAMPOA CHINESE MEDICINE
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