Method for quickly quantifying traditional Chinese medicine active components based on NMR technique

A technology for active components and traditional Chinese medicines, applied in the field of rapid quantification of active components of traditional Chinese medicines, can solve problems such as inability to find internal standard compounds, large differences in correction factors, etc., to achieve quantitative comparison, reduce time consumption and cost, and quickly batch effect achieved

Active Publication Date: 2017-11-24
XIAN UNIV OF SCI & TECH
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Problems solved by technology

When the content is determined by the external standard method, a standard sample is also required to draw a standard curve, and its disadvantages are the same as those of HPLC-UV
When the internal standard method is used, no standard is required, but the calibration factor of the internal standard is the same as that of the measured substance. Due to the limitation of the principle of MS, under the same conditions, the ionization degree of different structural types of compounds is very different. Calibration The factors are also very different, and it is impossible to find a single internal standard for the simultaneous determination of compounds of different structure types

Method used

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  • Method for quickly quantifying traditional Chinese medicine active components based on NMR technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Quantitative analysis of iridoids in Gentiana quinquefolium extract

[0029] The traditional Chinese medicine Gentiana chinensis is widely used clinically, and it is one of the main medicines for treating rheumatic arthralgia, tuberculosis hot flashes, jaundice, etc. The iridoids are the main active ingredients of the traditional Chinese medicine Gentiana chinensis.

[0030] (1) Quantitative analysis steps and results

[0031] Gentiana chinensis extract (Xi'an Tianrui Biological Company, 75% ethanol extract) 100mg was dissolved in 0.5mL deuterated chloroform (CDCl 3), transferred to a 5mm standard NMR tube, and then added 5 μL of trichlorethylene solution (solvent is deuterated chloroform, 1M), Bruker 400MHz to measure the hydrogen resonance signal of the sample, the temperature of the probe is controlled at 24°C, and the pulse sequence zg (90 degree pulse angle) is called , redefine relaxation time d1=5s, number of scans ns=32; Other parameters are standard...

Embodiment 2

[0039] Example 2 Quantitative Analysis of Paeoniflorin Compounds in Guizhi Fuling Pills

[0040] The prescription of Guizhi Fuling Pills comes from "Synopsis of the Golden Chamber" written by Zhang Zhongjing in the Eastern Han Dynasty. It is currently a commonly used medicine for treating gynecological blood stasis diseases. Paeoniflorin compounds are not only its active ingredients but also one of the key factors for quality control.

[0041] (1) Quantitative analysis steps and results

[0042] Guizhi Fuling pills 20mg dissolved in 0.5mL deuterated methanol (CD 3 OD), transferred to a 5mm standard NMR tube, then added 10 μL of pentafluorobenzene solution (solvent is deuterated methanol, 0.1M), Bruker 400MHz to measure the hydrogen resonance signal of the sample, the temperature of the probe was controlled at 40°C, and the pulse sequence zg30 (30°C pulse angle), redefine the relaxation time d1=5s, and the number of scans ns=1024; other parameters are standard parameters in t...

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Abstract

The invention provides a method for quickly quantifying traditional Chinese medicine active components based on a NMR (Nuclear Magnetic Resonance) technique. The method comprises the following steps: 1) dissolving a sample in a deuterium-substituting reagent, transferring into a nuclear magnetism tube and adding an internal standard substance into the nuclear magnetism tube; 2) sampling by adopting hydrogen resonant frequency in NMR; and 3) selecting a feature structure signal peak and an internal standard substance signal peak of a to-be-measured component and quantifying and calculating the content of the to-be-measured component by adopting an internal standard method. The method selects the NMR technique to detect the content of the traditional Chinese medicine active components, is capable of quickly quantitative analyzing the active components, such as, Chinese herb extracts, primary separating compounds or mixture thereof and natural sourced small molecule compounds, and is capable of giving the mole content. The method has the characteristics of simple operation, quick batch realization, high test reproducibility, direct and reliable test data, and the like; the method is especially suitable for the detection for trace sample; and a quick quantifying thought and a quick quantifying method are supplied for the research on the traditional Chinese medicine or compound effective material basis.

Description

technical field [0001] The invention relates to a method for rapidly quantifying active components of traditional Chinese medicine based on NMR technology, which belongs to the field of traditional Chinese medicine. Background technique [0002] The research on the material basis of pharmacodynamics of traditional Chinese medicine is the core issue in the process of modernization of traditional Chinese medicine. The traditional "separation-identification-screening" natural medicinal chemistry research model has a large workload and low separation efficiency; at the same time, the characteristics of complex components and relatively low content of medicinal substances increase the difficulty of research on medicinal substances and limit the modernization of traditional Chinese medicine. pace of. At the same time, the structure-activity relationship research of modern pharmacology needs to clearly know the content of the active substance. The activity-oriented in vitro rapid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 陈福欣龚频陈苏英侯彬彬严贝贝
Owner XIAN UNIV OF SCI & TECH
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