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Method for determining contents of atractylenolide II and atractylenolide III in atractylodes macrocephala medicinal material

A technique of atractylodes lactone and determination method, which is applied in the directions of measuring device, material separation, analysis material, etc., can solve the problems of long peak time, no content measurement items, and analysis of atractylide II.

Pending Publication Date: 2021-06-15
青海普兰特药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Atractylodes atractylodes has strong clinical application value and broad market demand, but the 2015 edition of Chinese Pharmacopoeia does not contain content determination items, which cannot comprehensively evaluate the quality of Atractylodes atractylodes
The current literature research reports about the content of Atractylodes macrolide in Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Lactone content mostly adopts HPLC method, adopts gradient elution procedure to carry out separation, and gradient elution is exactly two or more different polarity but miscible solvents, change with time Mix according to a certain ratio to continuously change the polarity of the washing solution, so that complex components can be well separated, but the following technical problems exist in the results of this gradient elution procedure: long peak eluting time, poor resolution, bad peak shape, Poor reproducibility, poor stability, large solvent consumption, low accuracy, etc.
[0005] The technical problem in the application number CN201910299616.6 is to study the characteristic maps of Baizhu decoction pieces, bran-fried Atractylodes decoction pieces, Atractylodes standard decoction and bran-fried Atractylodes standard decoction, but not for the content determination of Atractylodes lactone II and Atractylodes lactone III For analysis, and the method takes a long time to get out of the peak, the peak shape is not good, the resolution is poor, and the stability is poor
[0007] Technical problems in the application number CN201910725324.4: This application is aimed at the detection of Atractylodes I and Atractylodes III, but does not analyze Atractylides II, and the target peak separation of this method is not good, the reproducibility and accuracy are poor Low
[0009] Technical problems in application number CN202010678723.2: This application is aimed at the detection of Atractylodes lactone I and Atractylodes lactone III, but does not analyze Atractylodes lactone II, and the method is complicated to operate, the chromatographic peaks are not well separated, and the peak time is slow , poor stability, large solvent consumption, low accuracy

Method used

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  • Method for determining contents of atractylenolide II and atractylenolide III in atractylodes macrocephala medicinal material
  • Method for determining contents of atractylenolide II and atractylenolide III in atractylodes macrocephala medicinal material
  • Method for determining contents of atractylenolide II and atractylenolide III in atractylodes macrocephala medicinal material

Examples

Experimental program
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Effect test

Embodiment 1

[0078] [Determination of Atractylodes lactone Ⅱ and Atractylodes lactone Ⅲ] Determination according to high performance liquid chromatography (general rule 0512)

[0079] Preparation of the test solution: Take 0.5g of Atractylodes macrocephala powder, accurately weigh it, put it in a stoppered conical flask, add 50ml of 70% methanol accurately, weigh it, ultrasonically treat it for 10min, let it cool, weigh it again, and use 70 Make up the lost weight with % methanol, shake well, centrifuge at a frequency of 10000r / min for 5min, filter, and take the filtrate to obtain the final product;

[0080] Preparation of reference substance solution: Take appropriate amount of Atractylodes lactone II reference substance and Atractylodes lactone III reference substance, weigh them accurately, add 70% methanol to make solutions containing 10ug of Atractylodes lactone II and 10ug of Atractylodes lactone III per 1ml, to obtain ;

[0081] Chromatographic conditions and system suitability tes...

Embodiment 2

[0084] [Determination of Atractylodes lactone Ⅱ and Atractylodes lactone Ⅲ] Determination according to high performance liquid chromatography (general rule 0512)

[0085] Preparation of the test solution: take 0.5g of Atractylodes macrocephala powder, accurately weigh it, put it in a stoppered conical flask, add 50ml of 30% methanol accurately, weigh it, ultrasonically treat it for 20min, let it cool, weigh it again, and use 30 Make up the lost weight with % methanol, shake well, centrifuge at 8000r / min for 2min, filter, and take the filtrate to obtain the final product;

[0086] Preparation of reference substance solution: Take appropriate amount of Atractylodes lactone II reference substance and Atractylodes lactone III reference substance, weigh them accurately, add 70% methanol to make solutions containing 10ug of Atractylodes lactone II and 10ug of Atractylodes lactone III per 1ml, to obtain ;

[0087] Chromatographic conditions and system suitability test: the chromatog...

Embodiment 3

[0090] [Determination of Atractylodes lactone Ⅱ and Atractylodes lactone Ⅲ] Determination according to high performance liquid chromatography (general rule 0512)

[0091] Preparation of the test solution: take 0.5g of Atractylodes macrocephala powder, accurately weigh it, put it in a stoppered conical flask, accurately add 50ml of 50% methanol, weigh it, ultrasonically treat it for 30min, let it cool, weigh it again, and use 50 Make up the lost weight with % methanol, shake well, centrifuge at a frequency of 12000r / min for 8min, filter, and take the filtrate to obtain the final product;

[0092] Preparation of reference substance solution: Take appropriate amount of Atractylodes lactone II reference substance and Atractylodes lactone III reference substance, weigh them accurately, add 70% methanol to make solutions containing 10ug of Atractylodes lactone II and 10ug of Atractylodes lactone III per 1ml, to obtain ;

[0093] Chromatographic conditions and system suitability tes...

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Abstract

The invention relates to a method for determining the contents of atractylenolide II and atractylenolide III in an atractylodes macrocephala medicinal material, which comprises the following steps of: taking the atractylodes macrocephala medicinal material, extracting by using 70% methanol, carrying out gradient elution by using an acetonitrile-0.1% phosphoric acid water system, and determining the contents of atractylenolide II and atractylenolide III in the atractylodes macrocephala medicinal material. According to the method, on the basis of a rhizoma alismatis decoction detection method, through optimization of a series of research on mobile phase proportion gradient, detection wavelength, an extraction solvent, an extraction mode, extraction time and a chromatographic column, the result shows that the peak time is short, the peak shape is good, the separation degree and the peak purity are qualified, the accuracy is high and the stability is good, the operation is simple, convenient and rapid, the quality detection method of the atractylodes macrocephala medicinal material is perfected, so that the quality is better controlled.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and in particular relates to a content determination method for atractylodes lactone II and atractylodes lactone III in Atractylodes macrocephala medicinal materials. Background technique [0002] Atractylodes atractylodes is the rhizome of Atractylodes atractylodes perennial herbaceous plant. It is a very commonly used tonic Chinese medicine in Chinese medicine. It has the reputation of "Southern Art and Northern Ginseng". Atractylodes Rhizoma Atractylodes Rhizome is warm in nature, sweet in taste, slightly pungent and bitter, and enters the spleen and stomach meridians. Clinically, it is mainly used to invigorate the spleen. Diarrhea, phlegm retention, dizziness and palpitations, spontaneous sweating, restless fetal movement and other symptoms. In the past ten years, studies have shown that Atractylodes macrocephala has some effects in diuretic, anti-tumor, anti-bacterial, anti-inflammat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/74G01N30/86G01N30/88
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/74G01N30/8634G01N30/8679G01N30/88G01N2030/884
Inventor 郭静张学花邢会香王飞刘红余梅王周霞曹得辉杨恋
Owner 青海普兰特药业有限公司
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