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Method for controlling quality of radix scutellariae medicinal materials

A quality control method and technology of medicinal materials, applied in the direction of pharmaceutical formulas, medical preparations containing active ingredients, plant raw materials, etc., can solve problems such as easy formation of peaks, narrow distribution range, unfavorable samples, etc.

Inactive Publication Date: 2009-12-23
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The advantages of liquid chromatography detection method are: liquid chromatography has good objectivity and good resolution, and the investment in one-time instrument purchase is relatively small, but this method is a biased and selective detection method that requires intervention in the sample and destructive, which is not conducive to in vivo and in situ analysis; more complex preparation of samples is required and the throughput is limited; it is quite difficult to characterize (determine the structure) of unknowns; the repeatability of the method is average
The disadvantages of the liquid chromatography detection method are: there are certain problems in the resolution of the chromatography, the stability or reproducibility before and after the injection of the chromatographic column, and the qualitative (confirmation of the structure) of the unknown, etc., which need to be solved urgently.
[0003] At present, the research on the fingerprints of traditional Chinese medicines mainly focuses on the hydrogen nuclear magnetic resonance spectrum ( 1 HNMR) fingerprints, this is mainly because the amount of sample required for fingerprints is also very small, the scanning time is short, and it is easy to obtain, so it is widely used; but because 1 The narrow range of HNMR spectrum distribution results in 1 The overlapping peaks of the HNMR spectrum increase significantly, and it is easy to form wrapping peaks, which makes it difficult to distinguish and identify the characteristic signals

Method used

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  • Method for controlling quality of radix scutellariae medicinal materials
  • Method for controlling quality of radix scutellariae medicinal materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: a kind of method that Scutellaria baicalensis medical material fingerprint is established, it is to take the following steps:

[0024] (1) Establishment of standard Scutellaria baicalensis fingerprint

[0025] Preparation of standard Scutellaria baicalensis characteristic extract:

[0026] Take 5 g of standard Scutellaria baicalensis, add 50 mL of 95% ethanol, heat and reflux twice on a water bath, 1 hour each time, filter the extract, volatilize the solvent, and leave the residue for later use.

[0027] Determination of fingerprints of standard Scutellaria baicalensis:

[0028] Accurately weigh 10.0 mg of the characteristic extract dried at 60°C for 4 hours in a nuclear magnetic test tube, and accurately measure 0.5mL DMSO-d 6 Put it in a nuclear magnetic test tube, shake well, and use it for testing. Measuring conditions: Measuring temperature 25°C, scanning times 8000 times, DMSO-d 6 As the solvent, the δ39.49 residual solvent peak was used as the i...

Embodiment 2

[0031] Example 2: (1) Preparation of characteristic extract of standard Scutellaria baicalensis medicinal material sample: Take 5 g of standard Scutellaria baicalensis medicinal material sample, add 50 mL of 95% ethanol, heat and reflux twice on a water bath, each time for 1 hour, filter the extract, and volatilize the solvent , the residue is set aside.

[0032](2) Preparation of characteristic extracts of standard Scutellaria baicalensis medicinal materials: Take 5 g of the test sample, add 50 mL of 95% ethanol, heat and reflux on a water bath twice for 1 hour each time, filter the extract, volatilize the solvent, and leave the residue for later use.

[0033] (3) Determination method: Accurately weigh 20.0 mg of various characteristic extracts dried at 60°C for 4 hours in a nuclear magnetic test tube, and accurately measure 0.5mL DMSO-d 6 Put it in a nuclear magnetic test tube, shake well, and use it for testing. Measuring conditions: Measuring temperature 25°C, scanning ti...

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Abstract

The invention relates to a method for controlling the quality of radix scutellariae medicinal materials, comprising the following steps: taking standard radix scutellariae medical materials, obtaining a nuclear magnetic resonance spectroscopy thereof, and using characteristic ingredients of the radix scutellariae to identify the characteristic peak of medicinal effective ingredients as the characteristic peak of the radix scutellariae; taking a radix scutellariae sample to be tested, adopting the same method as a preparation method, a test condition and a test method of the standard radix scutellariae medical materials to test, obtaining a fingerprint electropherogram, and comparing the nuclear magnetic resonance spectroscopy of the radix scutellariae medicinal materials to be tested with the fingerprint electropherogram of the standard radix scutellariae medical materials. According to the differences of characteristic resonance peaks of the fingerprint electropherogram between the radix scutellariae medicinal materials to be tested and the standard radix scutellariae medical materials and number of common characteristic resonance peaks, the radix scutellariae medicinal materials can be classified as the following grades: high-class products: N is greater than 20, first-class products: N is greater than and equal to 18 and is less than or equal to 20, second-class products: N is greater than or equal to 16 and is less than 18, qualified products: N is greater than or equal to 14 and is less than 16, and unqualified products: N is less than 14.

Description

technical field [0001] The invention relates to a quality control method of traditional Chinese medicine, in particular to a quality control method of scutellaria baicalensis medicinal material, and also relates to the NMR fingerprint spectrum of the scutellaria baicalensis medicinal material obtained by the method. Background technique [0002] At present, the identification of Scutellaria baicalensis is often carried out by selecting one or two active components or index components of Scutellaria baicalensis for content determination, and judging the quality by its content. If only one or two active components of Scutellaria baicalensis are used to judge the internal quality of Scutellaria baicalensis, it is somewhat one-sided, not to mention the index components that have no medicinal effect. To control the efficacy of Scutellaria baicalensis, one or two chemical components must not be targeted, but its substance group must be controlled as a whole. Therefore, it is neces...

Claims

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Application Information

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IPC IPC(8): A61K36/539G01N24/08A61K125/00
Inventor 孙庆雷林云良祝贺王晓程传格刘建华
Owner SHANDONG ANALYSIS & TEST CENT
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