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Phlegm-heat clearing injection fingerprint spectrum establishment method and fingerprint spectrum thereof

A technology of fingerprint spectrum and establishment method, which is applied to the establishment method of Tanreqing injection fingerprint spectrum and the field of fingerprint spectrum, can solve the problems of difficult to achieve effective separation, complex chemical composition and the like, and achieves stable results, good reproducibility, Avoid one-sided effects

Active Publication Date: 2019-08-30
SHANGHAI KAIBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the complex chemical composition of Tanreqing Injection, it is difficult to achieve effective separation by conventional liquid chromatography using ordinary octadecyl-bonded silica gel as a filler.

Method used

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  • Phlegm-heat clearing injection fingerprint spectrum establishment method and fingerprint spectrum thereof
  • Phlegm-heat clearing injection fingerprint spectrum establishment method and fingerprint spectrum thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The establishment method of Tanreqing injection fingerprint of embodiment 1 comprises the following steps:

[0056] 1. Instruments and reagents

[0057] Agilent 1290 high performance liquid chromatograph (Agilent Corporation, USA).

[0058] Reagents: Acetonitrile and methanol are chromatographically pure, and other reagents are analytically pure.

[0059] Caffeic acid, chlorogenic acid, baicalin, scutellarin, and wogonin were all purchased from China Institute for the Control of Pharmaceutical and Biological Products, neochlorogenic acid, cryptochlorogenic acid, 3,4-dicaffeoylquinic acid, 3, 5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid, and forsythiaside E were all purchased from Shanghai Tongtian Biotechnology Co., Ltd. Chrysin-7-O-glucuronide , Melaleucain-7-O-glucuronide were purchased from Jiangsu Yongjian Pharmaceutical Technology Co., Ltd.

[0060] Test drug: a total of 33 batches of Tanreqing Injection, the sample information is shown in Table 1:

[006...

Embodiment 2

[0075] 2. Chromatographic conditions: with octadecylsilane bonded silica gel as filler; with acetonitrile as mobile phase A, with 0.1% formic acid solution as mobile phase B, carry out gradient elution according to the provisions in Table 3 (after the peak is completed Wash the chromatographic column with a high proportion of acetonitrile), the flow rate is 0.8ml / min, the column temperature is 30°C, and the detection wavelength is 280nm.

[0076] Table 3 Gradient elution program

[0077] time (minutes) Mobile phase A(%) Mobile phase B(%) 0～5 95 5 5～7 95→89 5→11 7～18 89→86 11→14 18～27 86→71 14→29 27～31 71→20 29→80

Embodiment 3

[0079] 2. Chromatographic conditions: with octadecylsilane bonded silica gel as filler; with acetonitrile as mobile phase A, with 0.1% formic acid solution as mobile phase B, carry out gradient elution according to the provisions in Table 4 (after the peak is completed Wash the chromatographic column with a high proportion of acetonitrile), the flow rate is 0.8ml / min, the column temperature is 30°C, and the detection wavelength is 280nm.

[0080] Table 4 Gradient elution program

[0081] time (minutes) Mobile phase A(%) Mobile phase B(%) 0～6 95 5 6～9 95→90 5→10 9～20 90→83 10→17 20～28 83→75 17→25 28～31 75→20 25→80

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Abstract

The invention relates to the technical field of medicine detection, and in particular relates to a phlegm-heat clearing injection fingerprint spectrum establishment method and a fingerprint spectrum thereof; the phlegm-heat clearing injection is prepared from scutellaria baicalensis, bear gall powder, cornu gorais, honeysuckle and fructus forsythiae, and a phlegm-heat clearing injection fingerprint spectrum is established by detecting the phlegm-heat clearing injection components by adopting an ultra-high performance liquid chromatography method; the method specifically comprises the followingsteps of S1, preparing a reference substance solution: taking a proper amount of caffeic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, 3, 4-dicaffeoylquinic acid and 3, 5-dicaffeoylquinic acid, 4, 5-dicaffeoylquinic acid, forsythiaside D, baicalin, scutellarin, chrysin-7-O-glucuronide, oroxylin-7-O-glucuronide and a wogonin reference substance, and adding methanol to prepare a solution which is 20-50 [mu]g in 1ml. according to the phlegm-heat clearing injection fingerprint spectrum establishment method provided by the invention, the method is simple and convenient to operate, stable in result, high in reproducibility and high in precision.

Description

technical field [0001] The invention relates to the technical field of medical detection, in particular to a method for establishing a fingerprint of Tanreqing injection and the fingerprint thereof. Background technique [0002] At present, the quality standards of traditional Chinese medicine are not standardized and perfect, and the means of quality analysis and evaluation are still very backward, which cannot accurately reflect the quality status of existing traditional Chinese medicine, which has become an obstacle for Chinese medicine to go abroad and go to the world. The fingerprint of Chinese patent medicine refers to the concept of fingerprint identification in forensic medicine, and uses certain analytical methods to obtain a common peak spectrum that can reflect the characteristics of the medicinal material or drug after proper processing. Identify and identify the quality of medicinal materials or medicines through the analysis of common peak spectra to ensure tha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/06G01N30/74
CPCG01N30/06G01N30/74G01N30/8686
Inventor 季申张静娴张小利胡青毛秀红穆竟伟
Owner SHANGHAI KAIBAO PHARMA
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