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Method for measuring content of eighteen ingredients of Huangqi Jianzhong Wan (astragalus mongholicus pill for invigorating stomach and regulating middle warmer)

A technology for Astragalus and Zhongwan pills is applied in the field of determination of 18 components in Astragalus Jianzhong pills by ultra-high performance liquid chromatography tandem mass spectrometry, which can solve the problems of complex ingredients, unclear active substances, complex traditional Chinese medicine ingredients, etc., and achieves simple pretreatment and analysis. Short time, good separation effect

Inactive Publication Date: 2019-05-31
SHANXI UNIV
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0003] The composition of traditional Chinese medicine is very complex, the active substance is not clear, the content difference between components is large, and the detection of drug effect mechanism is difficult, which makes the quality control of traditional Chinese medicine more difficult.
Moreover, Chinese medicine compound preparation is the main form of traditional Chinese medicine, which is composed of multi-flavored Chinese medicinal materials, and the ingredients are more complex.

Method used

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  • Method for measuring content of eighteen ingredients of Huangqi Jianzhong Wan (astragalus mongholicus pill for invigorating stomach and regulating middle warmer)
  • Method for measuring content of eighteen ingredients of Huangqi Jianzhong Wan (astragalus mongholicus pill for invigorating stomach and regulating middle warmer)
  • Method for measuring content of eighteen ingredients of Huangqi Jianzhong Wan (astragalus mongholicus pill for invigorating stomach and regulating middle warmer)

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0021] (1) Preparation of the test solution: Take Huangqi Jianzhong Pills, add liquid nitrogen and quickly grind them to powder, accurately weigh 0.25g and 1.5g each in a centrifuge tube, add 1mL of methanol, vortex for 1min to mix, and carry out Sonicate for 20 minutes, centrifuge for 15 minutes under the condition of 13000r / min, take the supernatant, and obtain the test solution No. 1 and No. 2, which are respectively used for mass spectrometry positive and negative ion mode analysis;

[0022] (2) Preparation of reference solution: take formononetin, formononetin, acteosin, acteosin, pterostalane, pteroside, isoflavane, isoliquiritin, liquiritin, liquiritin, licorice times Acid, cinnamic acid, gallic acid, isoflavane, astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅲ and astragaloside Ⅳ reference substances were accurately weighed, placed in a 5mL volumetric flask, and methanol was added to make the concentrations 0.218mg / mL, 0.192mg / mL, 0.27mg / mL, 0.312mg / mL, 0.256mg / mL, 0....

Embodiment 2

[0029] Example 2 Investigation on the determination method of eighteen kinds of ingredients in Huangqi Jianzhong Pills

[0030] The need testing solution of following experiment all adopts following method preparation:

[0031] Take Huangqi Jianzhong Pills, add liquid nitrogen to quickly grind to powder, accurately weigh 0.25g and 1.5g, add methanol 1mL, ultrasonically extract for 20min, centrifuge at 13000r / min for 15min, take the supernatant, and filter through a 0.22μm microporous membrane , that is, the test solution was used for mass spectrometry positive and negative ion mode analysis.

[0032] 1) Establishment of standard curve and linear range test

[0033] Dilute the mixed standard solutions A and B to the respective final concentrations of 80%, 66%, 33%, 12.5%, 5%, 2% of the serial concentrations, using the proposed method, using Waters ACQUITY UPLC HSS T3 (2.1mm ×100mm, 1.8μm) chromatographic column was detected by Agilent 1290 ultra-high performance liquid chroma...

example 3

[0051] Example 3 Detection of Eighteen Components in Huangqi Jianzhong Pills

[0052] Utilize the determination conditions of the eighteen kinds of ingredients established above to measure Huangqi Jianzhong Pills:

[0053] Take Huangqi Jianzhong pills respectively, add liquid nitrogen and quickly grind them to powder, accurately weigh 0.25g and 1.5g, add 1mL of methanol respectively, vortex for 1min to mix, perform ultrasonic treatment for 20min, centrifuge at 13000r / min for 15min, take the upper Clear, that is, the test solution No. 1 and No. 2.

[0054] Waters ACQUITY UPLC HSS T3 liquid chromatographic column, specification: 2.1mm×100mm, 1.8μm as stationary phase, was tested according to the following liquid phase conditions: column temperature was 45°C; injection volume was 5μL; flow rate was 0.25mL / min; acetonitrile and 0.2% formic acid water as the mobile phase.

[0055] Using MRM multiple reaction monitoring mode, ESI ion source, ion source temperature 400 ℃, mass ran...

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Abstract

The invention provides a method for measuring content of eighteen ingredients of Huangqi Jianzhong Wan (astragalus mongholicus pill for invigorating the stomach and regulating the middle warmer). Themethod includes the steps of subjecting the Huangqi Jianzhong Wan to ultrasonic extraction and centrifugation, extracting the liquid supernate, detecting the liquid supernate by an ultra performance liquid chromatography-tandem mass spectrometry positive and negative ion mode, preparing a mixed standard product solution from standard products of the eighteen ingredients, building a standard curve,and carrying out the methodological study. The method can realize measuring the eighteen ingredients of the Huangqi Jianzhong Wan, namely ononin, formononetin, calycosin, calycosin-7-glucoside, pterocarpan, astraisoflavan-7-O-beta-D-glucoside, isoflavane, isoliquiritin, liquiritigenin, liquiritin, glycyrrhetinic acid, cinnamic acid, isomucronulatol 7-O-beta-glucoside, astragaloside I, astragaloside II, astragaloside III, astragaloside IV and gallic acid. In the method, the sample pre-treatment process is simple and accordingly time for measurement is short; the method has the advantages of high specificity, high flexibility, good reproducibility and short analysis time, and can be applied to monitoring of production quality of the Huangqi Jianzhong Wan.

Description

technical field [0001] The invention relates to the technical field of detection of traditional Chinese medicine components, in particular to a method for determining 18 components in Huangqi Jianzhong Pills by ultra-high performance liquid chromatography tandem mass spectrometry. Background technique [0002] Huangqi Jianzhong Pill is derived from Zhongjing Jingfang Huangqi Jianzhong Decoction. The whole prescription is composed of five herbs of Astragalus, cinnamon, white peony root, roasted licorice and jujube. Clinically, it is mainly used to invigorate qi and dispel cold, invigorate the stomach and harmonize the middle. Insufficient Qi, shortness of breath, aversion to cold, abdominal pain and weakness. Modern pharmacological studies have shown that it is effective in treating gastrointestinal diseases caused by spleen deficiency; in addition, studies have shown that Huangqi Jianzhong Pills also have sedative and antispasmodic effects, lowering blood sugar, regulating ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 刘月涛贾璐秦雪梅
Owner SHANXI UNIV
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