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HPLC (High Performance Liquid Chromatography) fingerprint spectrum establishment method for Yixuean granules

A fingerprint and method establishment technology, which is applied in the field of drug detection, can solve the problems that the research on fingerprint establishment methods is still relatively small, and achieve the effects of short chromatographic analysis time, good reproducibility and stability, and quick and easy processing

Active Publication Date: 2016-07-20
广西万寿堂药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still relatively few studies on the establishment of fingerprints of Yixuan Granules.

Method used

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  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum establishment method for Yixuean granules
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum establishment method for Yixuean granules
  • HPLC (High Performance Liquid Chromatography) fingerprint spectrum establishment method for Yixuean granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] The optimization of embodiment 1 chromatographic conditions

[0067] The preparation method of the test solution: Weigh 5g of Yixuean granules, add 50mL of water to dissolve, add 0.3mL of dilute hydrochloric acid, stir well, let stand for 20min, filter, add water-saturated n-butanol to extract 5 times, each time 15mL, divide Take n-butanol extracts, combine them, let stand for 1h, separate to obtain n-butanol liquid, recover n-butanol, add 5 mL of methanol to the residue, centrifuge, and take supernatant to obtain the test solution.

[0068] 1-1 Selection of chromatographic column

[0069] The other determination conditions of the high performance liquid chromatography are the same. WelchromC18 column (4.6mm×250mm, 5μm), HypersilC18 column (4.6mm×250mm, 5μm) and PhenomenexGeminiC18 column (4.6mm×250mm, 5μm) three kinds of chromatographic columns were investigated. The resulting chromatograms are divided into figure 1 , figure 2 , image 3 shown by image 3 It can ...

Embodiment 2

[0078] The optimization of embodiment 2 sample pretreatment method

[0079] Chromatographic conditions of high-performance liquid chromatography: chromatographic column adopts Phenomenex GeminiC18 column (4.6mm * 250mm, 5 μ m); Guard column adopts PhenomenexC18 (4 * 3.0mm); Mobile phase: methanol-0.1% glacial acetic acid; Gradient elution program: time gradient

[0080] 0min→11min→16min→29min→30min→35min→45min→55min→70min→95min; the corresponding gradient elution solution is composed of mobile phase A methanol and mobile phase B 0.1% glacial acetic acid according to the following volume ratio, mobile phase A Volume percentage gradient 5%→16%→17%→30%→34%→34%→35%→45%→45%→70%, mobile phase B volume percentage gradient 95%→84%→83%→70 %→66%→66%→65%→55%→55%→30%;; detection wavelength: 256nm; flow rate: 1.0mL·min-1; column temperature: 25°C; injection volume: 5μL.

[0081] 2-1 Selection of extraction solvent

[0082] Weigh 5g of Yixuan granules, select water, methanol and ethanol ...

Embodiment 3

[0089] Example 3 Establishment of HPLC Fingerprint of Yixuan Granules

[0090] 3-1 Preparation of reference substance solution: Weigh 0.81mg of protocatechuic acid standard substance and place it in a 10mL volumetric flask, add an appropriate amount of methanol to dissolve it and set the volume to the mark, shake well, and obtain a solution with a concentration of 0.081mg·mL-1 Protocatechuic acid standard solution

[0091]3-2 Preparation of the test solution: Weigh 5g of Yixuan granules, add 50mL of water to dissolve, add 0.3mL of dilute hydrochloric acid, stir well, let stand for 20min, filter, add water and extract with n-butanol for 5 times, 15mL each time , separate the n-butanol extracts, combine them, let stand for 1h, separate and obtain the n-butanol liquid, recover the n-butanol, add methanol 5mL to the residue, centrifuge, and take the supernatant to obtain the test solution.

[0092] 3-3 Chromatographic conditions of high performance liquid chromatography:

[0093...

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Abstract

The invention discloses an HPLC (High Performance Liquid Chromatography) fingerprint spectrum establishment method for Yixuean granules. Protocatechuic acid is adopted as a reference, and gradient elution is performed to obtain a fingerprint spectrum of a common mode of medicinal materials of a Zhuang medicament blumea riparia by HPLC. The fingerprint spectrum has totally 21 chromatographic peaks, chemical components of the Yixuean granules can be completely reflected, the information amount is large, and the method is high in precision, reproducibility and stability and significant for quality control and clinical efficacy of the Yixuean granules.

Description

technical field [0001] The invention relates to the field of drug detection, in particular to a method for establishing HPLC fingerprints of Yixuan granules. Background technique [0002] Yixue'an Granule is a Chinese patent medicine for treating gynecological anemia. Clinically, it is used for persistent postpartum lochia, unclean uterine bleeding after artificial abortion, and blood stasis syndrome in TCM. [0003] With the application of new technologies and methods in recent years, many new ideas have appeared in the research of compound Chinese medicines. The use of fingerprints to study compound Chinese medicines is one of them. Fingerprints are of great significance to the quality control research and quality control standards of Chinese medicine compound . However, there are still relatively few studies on the establishment of fingerprints of Yixuan granules. [0004] The invention patent with the authorized notification number CN104458993B discloses a method for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 侯小涛李修善慕丽群毛金玲
Owner 广西万寿堂药业有限公司
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