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Method for detecting ultra-high performance liquid chromatography characteristic chromatogram of semen descurainiae formula granules

An ultra-high-efficiency liquid phase and formula granule technology, which is applied in the field of quality control of Tinglizi formula granules, can solve problems such as poor separation effect and feature map control, and achieve objective conclusions

Pending Publication Date: 2022-01-21
SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the 2020 edition of "Chinese Pharmacopoeia", the qualitative and quantitative control of Tinglizi chinensis is limited to its quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside. its characteristic map control
However, the separation effect between the chromatographic peaks of the characteristic spectra in the quality standards of traditional Chinese medicine formula granules in the above provinces is poor

Method used

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  • Method for detecting ultra-high performance liquid chromatography characteristic chromatogram of semen descurainiae formula granules
  • Method for detecting ultra-high performance liquid chromatography characteristic chromatogram of semen descurainiae formula granules
  • Method for detecting ultra-high performance liquid chromatography characteristic chromatogram of semen descurainiae formula granules

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0092] 3. Preparation of the test solution

[0093] (1) Selection of extraction solvent

[0094] Because the Tinglizi formula granule is concentrated from the water extract of Tinglizi, it has strong water solubility. The extraction effect of pure water, 25% methanol aqueous solution, 50% methanol aqueous solution, 75% methanol aqueous solution and 100% methanol on the Tinglizi formula granules was investigated, and the percentages here are methanol volume percentages.

[0095] The specific experimental method is as follows:

[0096] Take an appropriate amount of this product, grind it finely, take about 0.2g, accurately weigh it, put it in a stoppered Erlenmeyer flask, accurately add 25ml of different solvents, weigh it, ultrasonically treat it (frequency 37kHz, power 1130W) for 15 minutes, let it cool, Weigh again, make up the lost weight with different solvents, shake well, centrifuge at 12000rpm for 10 minutes, filter, and take the filtrate to obtain the final product. ...

Embodiment 1

[0225] Example 1: Detection of UPLC characteristic spectrum and establishment of control spectrum of Tinglizi formula granules

[0226] 1. Test method

[0227] 1.1 Preparation of the test solution: Take an appropriate amount of this product, grind it finely, take about 0.2g, accurately weigh it, put it in a stoppered Erlenmeyer flask, add 25ml of 25% methanol aqueous solution, weigh it, and ultrasonically treat it (power 37kHz , frequency 1130W) for 15 minutes, let cool, weigh again, make up the lost weight with 25% aqueous methanol solution, shake well, centrifuge at 12000rpm for 10 minutes, filter, and get the filtrate to get final product.

[0228] 1.2 Preparation of reference substance solution: Take an appropriate amount of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside reference substance, weigh it accurately, add 25% methanol water to make each 1ml containing 15μg of the solution, that is.

[0229] 1.3 Chromatographic conditions: using Waters ACQUITY HSS T3 (1.8μm,...

Embodiment 2

[0237] Example 2: Quality identification of Tinglizi formula granules

[0238] 1. Test method

[0239] 1.1 Preparation of reference substance solution: Take an appropriate amount of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside reference substance, accurately weigh it, add 25% methanol aqueous solution to make each 1ml containing 15μg of the solution, that is.

[0240] 1.2 Chromatographic conditions: using Waters ACQUITY HSS T3 (1.8μm, 2.1×100mm) chromatographic column, with acetonitrile as mobile phase A and 0.1% trifluoroacetic acid aqueous solution as mobile phase B, carry out gradient elution as specified in the table below; the flow rate is 0.3ml per minute; The column temperature is 30°C; the detection wavelength is 254nm.

[0241]

[0242] 1.3 Preparation of the test solution of the sample to be identified: Take an appropriate amount of the sample to be identified, grind it finely, take about 0.2g, accurately weigh it, put it in a stoppered Erlenmeyer flask, ad...

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Abstract

The invention relates to a method for detecting an ultra-high performance liquid chromatography characteristic spectrum of semen descurainiae formula granules, a method for establishing a contrast spectrum of the semen descurainiae formula granules and a quality control method of the semen descurainiae formula granules. The method for detecting the UPLC characteristic chromatogram of the semen descurainiae formula granules adopts an ultra performance liquid chromatograph for analysis, and chromatographic conditions are as follows: a chromatographic column adopts octadecylsilane chemically bonded silica as a filler, a mobile phase adopts acetonitrile as a mobile phase A, a 0.02-0.10% trifluoroacetic acid aqueous solution, preferably 0.1% trifluoroacetic acid aqueous solution as a mobile phase B, and gradient elution is performed; the flow rate is 0.20 to 0.40 ml per minute; the column temperature is 20-35 DEG C; the detection wavelength is 203 to 360 nm; the sample size is 2 microliters. The method provided by the invention provides a rapid and comprehensive detection means for the quality control of the descurainia seed formula granules.

Description

technical field [0001] The invention belongs to the technical field of quality control of Tinglizi formula granules, and relates to a method for detecting ultra-high performance liquid chromatography (UPLC) characteristic spectrum of Tinglizi formula granules, a method for establishing a control spectrum of Tinglizi formula granules, and Tinglizi formula granules. The quality control method of zizi formula granules. Background technique [0002] Tinglizi is the dried and mature seed of the cruciferous plant Artemisia persicae. It is recorded in the 2020 edition of "Chinese Pharmacopoeia" and is a commonly used traditional Chinese medicine. It has the effects of purging the lungs and relieving asthma, promoting water to reduce swelling; it is used for phlegm and saliva obstructing the lungs, wheezing and coughing with excessive phlegm, fullness of the chest and ribs, inability to lie on the back, edema of the chest and abdomen, and difficulty in urinating. [0003] The main ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/60
CPCG01N30/06G01N30/60
Inventor 果德安张建青李萍姚长良魏文龙
Owner SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI
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