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Construction method of <1>H-NMR fingerprint of radix astragali injection

A technology of astragalus injection and fingerprints, which is applied in the field of quality control of traditional Chinese medicine injections, and can solve problems such as difficult detection of chromatographic fingerprints

Active Publication Date: 2014-12-03
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since most of these components are highly polar substances that are poorly retained on the column, they are difficult to detect with existing chromatographic fingerprints

Method used

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  • Construction method of &lt;1&gt;H-NMR fingerprint of radix astragali injection
  • Construction method of &lt;1&gt;H-NMR fingerprint of radix astragali injection
  • Construction method of &lt;1&gt;H-NMR fingerprint of radix astragali injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 Astragalus Injection 1 Establishment of H-NMR Fingerprint

[0024] 1) Sample preparation:

[0025] ① Take 10ml of Astragalus injection and directly evaporate to dryness, take 50mg of dry powder, dissolve with deuterated methanol: heavy water = 1:1, transfer to a 1.5ml centrifuge tube, centrifuge at 13000rpm for 10 minutes, pipette 600μL of supernatant into a 5mm NMR tube , for Astragalus Injection 1 H-NMR fingerprint spectrum A analysis;

[0026] ② Take 30ml of Astragalus injection, add an equal volume of ethyl acetate to extract twice, combine the extracts, evaporate to dryness, add 800μL of deuterated methanol to dissolve, transfer to a 1.5ml centrifuge tube, centrifuge at 13000rpm for 10 minutes, and pipette 600μL of supernatant The solution is used in a 5mm NMR tube for Astragalus Injection 1 H-NMR fingerprint spectrum B analysis;

[0027] 2) Spectrum collection: The sample is measured on a 600MHz NMR instrument at 25°C, and the measurement frequen...

Embodiment 2

[0031] Embodiment 2 This method is used for the quality evaluation of Radix Astragali Injection

[0032] A total of 8 batches of Astragalus injection from 5 different manufacturers (denoted as: A, B, C, D, E) were collected (A manufacturer: 3 batches; B manufacturer: 1 batch; C manufacturer: 1 batch D producer: 1 batch; E producer: 2 batches), carry out according to the method determined in the content of the present invention 1 H-NMR analysis, obtained different manufacturers of Astragalus injection 1 H-NMR fingerprints A and B; segmented integration of fingerprint A (chemical shift range 0.34-10.02) and fingerprint spectrum B (chemical shift range 0.76-9.92) with δ0.04ppm, where δ4.80~5.06 (residual water peak) and δ3.30~3.34 (residual methanol peak) are not integrated, and the integrated data is imported into SIMCA-P 11.0 software for PCA (principal component analysis) and PLS-DA (partial least squares discriminant multiplication) analyze.

[0033] Astragalus Injection ...

Embodiment 3

[0034] Example 3 Relative Content Comparison of Primary Metabolites of Astragalus Injection from Different Manufacturers

[0035] Astragalus Injection 1 The H-NMR fingerprint spectrum A was analyzed, with TSP as the internal standard, and the relative content of 13 primary metabolites was calculated by the integral area. From Figure 5 It can be seen that there are large differences in the relative content and proportion of primary metabolites among different manufacturers. There are fewer types of primary metabolites in manufacturers B and C, and the relative content and proportion of 13 primary metabolites in different batches of Astragalus injection from the same manufacturer. The content and proportion are close. From Figure 6 It can be seen that the same primary metabolites are different among different manufacturers and different batches of the same manufacturer. It can be seen from this example that NMR fingerprints can be used to compare the homogeneity of primary...

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Abstract

The invention discloses a construction method of the <1>H-NMR fingerprint of a radix astragali injection, belonging to the field of quality control of traditional Chinese medicine injections. According to the construction method, the fingerprint and the characteristic peak of the fingerprint of the radix astragali injection are obtained by adopting the nuclear magnetic resonance technology, primary and secondary metabolites, namely totally 25 chemical components, in the radix astragali injection can be represented at the same time, the integral quality characteristic of the radix astragali injection can be accurately reflected, and thus the construction method can be used for quality control on radix astragali injection products and can ensure safe and effective clinical medication.

Description

technical field [0001] The present invention relates to the quality control method of traditional Chinese medicine injection, particularly a kind of astragalus injection 1 Construction method of H-NMR fingerprint. Background technique [0002] Astragalus Injection is a classic prescription recorded in Volume 17 of the Standards issued by the Ministry of Traditional Chinese Medicine, and the standard number is WS 3 -B-3335-98 is prepared from Astragalus membranaceus through water extraction and alcohol precipitation. It can be used for heart qi deficiency, viral myocarditis caused by blood stasis, heart insufficiency and hepatitis caused by spleen deficiency and dampness. [0003] In-depth research on the quality control methods of traditional Chinese medicine injections is of great significance to ensure its effectiveness and safety in clinical use. Astragalus injection contains a variety of chemical components, but the ministerial standard (WS 3 -B-3335-98) only stipula...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 李震宇曲婷丽张丽增张松秦雪梅
Owner SHANXI UNIV
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