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Quality control method for rhizoma polygonatum medicinal material

A technology of quality control method and measurement method, applied in the field of quality control of Rhizoma Polygonatum, can solve problems such as insufficient stability and reproducibility, and achieve the effects of good repeatability and stability, high quality of the map, and many color bands

Active Publication Date: 2019-11-05
HUNAN XINHUI PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The stability and reproducibility of the above method is not good enough

Method used

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  • Quality control method for rhizoma polygonatum medicinal material
  • Quality control method for rhizoma polygonatum medicinal material
  • Quality control method for rhizoma polygonatum medicinal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The content of the present invention includes the following methods,

[0033] 1. Preparation of the test solution. Take 1g of fine powder dried to constant weight at 60℃ in a 50ml Erlenmeyer flask, add 20ml of water for ultrasonic extraction for 1h; after high-speed centrifugation, take 10ml of the supernatant and place it in an evaporating dish After the water bath evaporates to dryness, add 10ml of 3mol / l hydrochloric acid to dissolve it, then put the evaporating dish on the 95℃ water bath to make it hydrolyze and caramelize as it evaporates to dryness; when the hydrochloric acid solution is completely evaporated to dryness, add 2ml dropwise to the evaporating dish Methanol is used to take away the residual hydrochloric acid, repeat twice; the evaporated residue is dissolved in 10ml methanol, centrifuged and filtered through a microporous membrane to obtain;

[0034] 2. Liquid phase conditions: Agilent 1200LC high performance liquid chromatograph (equipped with G1311 quate...

experiment example 1

[0037] HPLC characteristic map

[0038] The extracts of Polygonatum with methanol, acetone, ether and other solvents were analyzed by HPLC. The sample preparation method was to take 2g of Polygonatum sample powder dried to constant weight at 60℃, and add 20ml of extraction solvent (the extraction solvents were methanol, acetone and Diethyl ether), ultrasonic extraction for 30min, take methanol to extract the supernatant, centrifuge at high speed, pass through a microporous membrane, sample analysis, take acetone and diethyl ether to extract the supernatant, centrifuge and take 12ml, spin dry with 1ml methanol Dissolve, centrifuge at high speed and take the supernatant through a microporous membrane, and then sample for analysis. Detection wavelength: 210nm; column temperature: 30°C; mobile phase: ACN / 0.05% H3PO4-H2O; elution conditions: 0-45min: 20-90% ACN, 45-50min: 90-95% ACN, 55-65min: 95% ACN; injection volume: 10μl, the HPLC chromatogram is as follows Figure 3-5 Shown. F...

experiment example 2

[0040] The Polygonatum polysaccharide is hydrolyzed, and then the hydrolyzed monosaccharide is derivatized for liquid phase analysis. The specific method is as follows.

[0041] Preparation of Polygonatum Polysaccharide: Take 1g of Polygonatum sample into a 50ml Erlenmeyer flask, add 20ml of water, ultrasonically extract for 45min, centrifuge to take the supernatant, add 80ml of absolute ethanol, put it in a refrigerator at 4℃ for 12h, centrifuge, and dissolve the precipitate with 10ml of water , Centrifuge to take the supernatant and spin-dry with a rotary evaporator to obtain Polygonatum polysaccharide.

[0042] Polysaccharide hydrolysis: Take the polysaccharide prepared above, dissolve it in a test tube with a stopper with 2ml of water, add 4ml of 2mol / L trifluoroacetic acid (TFA) solution, close it, hydrolyze it in an oven at 105°C for 6h, take it out and use a rotary evaporator Spin to dry, wash the precipitate with MeOH (3ml) and spin to dry, repeat 3 times to take away exces...

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Abstract

The invention relates to a quality control method for a rhizoma polygonatum medicinal material. The method comprises the following steps of a construction method of an HPLC fingerprint spectrum of therhizoma polygonatum medicinal material, a thin layer chromatography analysis method, a water content and total ash content measurement method and an extractum and total saponin measurement method; the construction method of the HPLC fingerprint spectrum of the rhizoma polygonatum medicinal material comprises the step of preparation of a test solution, wherein fine rhizoma polygonatum powder is collected, water is added for ultrasonic treatment, centrifugation is conducted, and a supernate is collected; after evaporation to dryness is conducted, hydrochloric acid is added for dissolution, andwater bath treatment is conducted; methyl alcohol is dropwise added to take residual hydrochloric acid away; residues after being evaporated to dryness are dissolved with methyl alcohol, centrifugation and filtration through a microfiltration membrane are conducted, and the test solution is obtained; according to the construction method of the HPLC fingerprint spectrum of the rhizoma polygonatum medicinal material, the same peak value exists for different rhizoma polygonatum medicinal materials, the precision, repeatability and stability are good, the similarity, to a contrast spectrum, of thefingerprint spectrum is 0.99 or greater, and the HPLC fingerprint spectrum is good in separation degree and peak shape, the quality of three kinds of rhizoma polygonatum can be comprehensively reflected, and counterfeit medicinal products are identified based on the reason.

Description

Technical field [0001] The invention belongs to a quality control method of traditional Chinese medicine products, in particular to a quality control method of Polygonatum. Background technique [0002] Polygonatum is the dry rhizomes of Polygonatum sibiricum Red., Polygonatum kingianum Coll.et Hemsl., Polygonatum cyrtonema Hua., which belong to the genus Polygonatum in the Liliaceae family. The fingerprint of traditional Chinese medicine can accurately reflect the true quality of traditional Chinese medicine and its preparations due to its integrity, vagueness and macroscopic characteristics. [0003] When selecting the specific HPLC fingerprint chromatographic conditions, the general principle is that the selected chromatographic conditions are to allow the various active ingredients contained in traditional Chinese medicine to appear in the spectrum to the maximum extent and the resolution is up to standard, and the peak shape is good. . [0004] When selecting the mobile phase,...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/86G01N30/90G01N21/31G01N33/15
CPCG01N21/31G01N30/8686G01N30/88G01N30/90G01N33/15G01N2030/8809
Inventor 何述金王炜袁汉文周准周代俊
Owner HUNAN XINHUI PHARMA
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