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Fingerprint construction and quality detection method of chrysanthemum broken wall decoction pieces

A technology of broken-walled decoction pieces and fingerprints, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of incomplete reflection of the quality of decoction pieces, specificity, stability, reproducibility, and poor precision, and achieve simple operation , Detection of fast and accurate results

Active Publication Date: 2016-08-24
ZHONGSHAN ZHONGZHI PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are detection methods involving the fingerprints of traditional Chinese medicines in the prior art, there is no method for broken-walled decoction pieces of traditional Chinese medicines with special morphology, and there are defects in specificity, stability, reproducibility and precision, which cannot fully reflect the decoction pieces. defect in quality

Method used

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  • Fingerprint construction and quality detection method of chrysanthemum broken wall decoction pieces
  • Fingerprint construction and quality detection method of chrysanthemum broken wall decoction pieces
  • Fingerprint construction and quality detection method of chrysanthemum broken wall decoction pieces

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Experimental program
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Effect test

experiment approach 1

[0031] Pre-experimental plan 1 Sample preparation: Accurately weigh 0.5146g of broken chrysanthemum decoction pieces, add 25ml of 75% methanol, weigh the weight, extract by ultrasonic for 40min, take it out, cool to room temperature, make up the weight with extraction solvent, coarse filter, and use 0.22um micro Pore ​​membrane filtration, take the continued filtrate, that is. Chromatographic conditions: Waters Symmetry C18 column (250mmx4.6mm, 5um); mobile phase is acetonitrile-0.5% phosphoric acid aqueous solution, gradient elution: 0min-1min-18min-32min-55min-75min, acetonitrile change 5%-10%- 18%-18%-25%-45%; flow rate 1ml / min; column temperature 35°C; detection wavelength 268, 351, 210nm; injection volume 10ul.

experiment approach 2

[0032] Pre-experimental scheme 2 Sample preparation: Accurately weigh 0.5146g of broken chrysanthemum decoction pieces, add 25ml of 75% methanol, weigh the weight, extract by ultrasonic for 40min, take it out, cool to room temperature, make up the weight with extraction solvent, filter roughly, and use 0.22um micro Pore ​​membrane filtration, take the continued filtrate, that is. Chromatographic conditions: Waters Symmetry C18 chromatographic column (4.6x250mm, 5um); mobile phase is acetonitrile-0.5% phosphoric acid aqueous solution, gradient elution: 0min-50min-100min, acetonitrile change: 10%-25%-60%; detection wavelength 268, 351, 210nm; flow rate 1ml / min; column temperature 30°C; injection volume 10ul.

experiment approach 3

[0033] Pre-experimental scheme 3 Sample preparation: Precisely take 0.5146g of broken-walled decoction pieces, add 25ml of 75% methanol, weigh the weight, extract by ultrasonic for 40min, take it out, cool to room temperature, make up the weight with extraction solvent, coarse filter, and use 0.22um microporous filter Membrane filtration, take the continued filtrate, that is. Chromatographic conditions: Waters Symmetry C18 column (250nmx4.6nm, 5um); mobile phase is acetonitrile-0.5% phosphoric acid aqueous solution, gradient elution: 0min-60min, acetonitrile change 5%-95%; flow rate 1ml / min; column temperature 35 ℃; detection wavelength 268, 351, 210nm; injection volume 10ul.

[0034] Pre-experiment 4 Sample preparation: Accurately weigh about 0.5146g of broken chrysanthemum decoction pieces, add 25ml of 75% methanol, weigh the weight, extract by ultrasonic for 40min, take it out, cool to room temperature, make up the weight with extraction solvent, filter roughly, and use 0.2...

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Abstract

The invention relates to a finger-print spectrum mutual mode construction method and a quality detection method of chrysanthemum cell-disruption decoction pieces. In the method, with isochlorogenic acid A as a contrast peak, mutual mode standard spectrums and determination indexes are established through HPLC analysis to not less than 10 batches of the samples under following chromatographic conditions: column temperature: 35 DEG C; wavelength: 348 nm; mobile phase: an acetonitrile-0.5% phosphoric acid solution; elution gradient: 0-8 min-24 min-50 min-75 min; and acetonitrile change: 14%-18%-18%-25%-45%. The spectrums of the samples to be detected under the same chromatographic condition are compared with the mutual mode standard spectrums to detect the quality of the samples to be detected. The invention firstly discloses the HPLC finger-print spectrum and the quality detection method aiming to the chrysanthemum cell-disruption decoction pieces. The spectrums comprehensively contain the spectrum information of main active components of the chrysanthemum cell-disruption decoction pieces. The method is strong in specificity, is quick and accurate in detection, and can effectively control the total quality of medicines, cell-disruption powders and cell-disruption decoction pieces.

Description

technical field [0001] The invention relates to a quality detection method of traditional Chinese medicine decoction pieces, in particular to the construction of HPLC fingerprint standard spectrum of broken-walled chrysanthemum decoction pieces and its quality detection method. Background technique [0002] Chrysanthemum is the dry flower head of Chrysanthemum morifolium Ramat. Traditional Chinese medicine wall-broken decoction pieces use modern ultrafine pulverization technology to break the cell wall of traditional decoction pieces into fine particles with a particle size distribution D90 of less than 45 μm, and then make 30-100 mesh particles. Compared with traditional decoction pieces, it has the characteristics of consistent color, uniform quality and good stability, which is an innovative Chinese medicine decoction piece. Since the broken pieces of traditional Chinese medicine do not have the morphological characteristics of traditional Chinese medicine pieces, the di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 王慧玲彭丽华徐吉银成金乐
Owner ZHONGSHAN ZHONGZHI PHARMA GRP
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