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Method for detecting and controlling fingerprint spectrum of Xiebai powder reference sample

A standard fingerprint, benchmark sample technology, applied in the field of quality control and detection of traditional Chinese medicine preparation and its components, can solve separation difficulties, limited content of the active ingredients of Chenyao Digupi, and the degree of separation of Digupitin is not up to standard, etc. question

Active Publication Date: 2021-09-10
SPH XING LING SCI & TECH PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the invention patent application with the application number "201811344359.5" provides a method for determining the content of Xiebai powder, but it only measures the contents of molaritin A, liquiritin, and ammonium glycyrrhizinate in Xiebai powder, and does not affect the content of the drug. The content of active ingredients in Digupi is limited
Another example is the invention patent application with the application number "202010666660.9", which provides a UPLC method for detecting the content of dichoticin and molaritin A in Xiebaisan granules, but only detects molarin A, The content of dicortin, and the separation degree of dicortin in this method did not meet the standard
Since dicortin and dicortin are isomers, it is difficult to separate them. At present, there is no literature on the content determination of dicortin and dicortin in Xiebai powder at the same time, and there is no Xiebai powder. In the report of the Baisan fingerprint, the literature that separated and identified dikosin and dikosin
It can be seen that the above-mentioned patent is not comprehensive in the detection of the components in the reference sample of Xiebaisan

Method used

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  • Method for detecting and controlling fingerprint spectrum of Xiebai powder reference sample
  • Method for detecting and controlling fingerprint spectrum of Xiebai powder reference sample
  • Method for detecting and controlling fingerprint spectrum of Xiebai powder reference sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0115] In parts by weight, accurately weigh 3.93g of fried mulberry bark, 3.93g of Digupi, 0.39g of roasted licorice, and 1g of japonica rice. After mixing, add two small cups of water to make 120mL. After boiling for 10 minutes, heat and decoct at 110°C for 10 minutes on a slow fire to form "fried seven minutes", to 84mL, and filter and extract with 100-mesh nylon cloth to obtain a water extract.

[0116] Precisely measure 5mL of the water extract, put it into a 10mL brown ampoule, freeze at -80°C for 12h in a lyophilizer, and dry at 25°C for 48h to obtain Xiebaisan sample 1#.

Embodiment 2

[0118] In parts by weight, accurately weigh 3.90g of fried mulberry bark, 3.90g of Digupi, 0.39g of roasted licorice, and 1g of japonica rice. After mixing, add two small cups of water to make 120mL. After boiling for 15 minutes, heat and decoct at 100°C for 15 minutes on a slow fire to form "fried seven minutes", to 84mL, filter and extract with 100-mesh nylon cloth to obtain a water extract.

[0119] Precisely measure 5mL of the water extract, put it into a 10mL brown ampoule, freeze at -60°C for 13h in a lyophilizer, and dry at 20°C for 50h to obtain Xiebaisan sample 2#.

Embodiment 3

[0121] 1. Solution preparation

[0122] Get the 5mL Xiebai San water extract prepared in Example 1 and freeze-dry the Xiebai San sample 1#, add 5mL water to redissolve, accurately pipette 1mL into a 2mL volumetric flask, dilute to the mark with methanol, and use 10000rpm Speed ​​centrifugation 5min, through 0.22μm microporous membrane, that is, the test solution 1#.

[0123] A reference substance solution is provided, and the reference substance solution includes disanbaritin A, chlorogenic acid, dicortexin, dicortexin, liquiritin, liquiritin, ammonium glycyrrhizinate reference substance and methanol.

[0124] 2. Chromatographic conditions

[0125] The chromatographic conditions of high performance liquid chromatography are: chromatographic column: Agilent Zorbax SB-Aq chromatographic column (250mm * 4.6mm, 5 μ m); Detector is photodiode array detector (DAD); Column temperature: 25 ℃; Detection wavelength: 273nm; Flow rate: 1.0mL / min; Injection volume: 20μL; Mobile phase: 0....

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Abstract

The invention provides Xiebai powder. The invention further provides a preparation method and an application of a Xiebai powder reference sample (substance reference). The invention also provides a method for detecting the fingerprint spectrum of the Xiebai powder reference sample. The invention further provides a construction method of the standard fingerprint spectrum of the Xiebai powder and a quality control method of the fingerprint spectrum of the Xiebai powder. In addition, the invention provides a method for detecting the contents of kukoamine B and kukoamine A in the Xiebai powder. According to the method for detecting and controlling the fingerprint spectrum of the Xiebai powder reference sample, the Xiebai powder reference sample with excellent quality can be obtained, the quality is stable, the reject ratio is low, the high performance liquid fingerprint spectrum of the Xiebai powder is also established, the internal quality of the Xiebai powder can be integrally controlled favourably, and a scientific test basis is provided for better establishing an overall quality control and evaluation system of the Xiebai powder.

Description

technical field [0001] The invention belongs to the technical field of preparation of traditional Chinese medicine and the quality control and detection of its components, and relates to a method for detecting and controlling the fingerprint of a reference sample of Xiebai powder; in particular, it relates to a preparation method of reference sample of Xiebai powder and the reference sample of Xiebai powder , the detection method of the fingerprint chromatogram of Xiebai powder reference sample, the construction method of the standard fingerprint chromatogram of Xiebai powder, the quality control method of the fingerprint chromatogram of Xiebai powder, digucortin and digucortin in Xiebai powder method for the determination of content. Background technique [0002] "Material standards of classic famous prescriptions" refers to the standards of medicinal substances of traditional Chinese medicine prepared on the basis of the preparation methods of classic famous prescriptions ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/8679G01N2030/047
Inventor 张彤高崎李婷王丹丹丁越朱国琴刘云江美芳
Owner SPH XING LING SCI & TECH PHARM CO LTD
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