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Method for detecting large-hole adsorbent resin organic matter residues in desmodium styracifolium general flavone extractive with headspace gas chromatography

A technology of headspace gas chromatography and Desmodium sativa, which is applied in the detection field of drug impurities in the new drug technology of traditional Chinese medicine, can solve the problems that need to be improved, and achieve the effect of short time, good accuracy and high detection sensitivity

Active Publication Date: 2015-09-23
WUHAN OPTICS VALLEY HUMANWELL BIO PHARMA
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Problems solved by technology

[0005] However, the current detection method for the residual limit of organic solvents in the macroporous adsorption resin in the total flavonoids extract of Desmodium stylifolia still needs to be improved

Method used

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  • Method for detecting large-hole adsorbent resin organic matter residues in desmodium styracifolium general flavone extractive with headspace gas chromatography
  • Method for detecting large-hole adsorbent resin organic matter residues in desmodium styracifolium general flavone extractive with headspace gas chromatography
  • Method for detecting large-hole adsorbent resin organic matter residues in desmodium styracifolium general flavone extractive with headspace gas chromatography

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Embodiment 1

[0070] The inventor carried out experimental verification to the residual solvent analysis method of the present invention, wherein each experiment adopts the method and detection parameters in the "general method" to carry out residual solvent detection and analysis, and the specific verification tests and results are as follows:

[0071] 1. System suitability

[0072] 1.1 Introduction

[0073] Investigate the system suitability at the beginning of each sequence, the blank solution has no interference peak; the system suitability is measured by repeating the RSD of each solvent peak area in the standard solution 6 times (that is, the standard solution prepared above is taken 6 parts and moved to 6 tops respectively). Empty sampling vials, measured 6 times respectively), and each solvent in the chromatogram obtained by 6 times is required ("each solvent" here corresponds to each component in the standard solution, and refers to each component to be measured, that is, The rela...

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Abstract

The invention discloses a method for detecting large-hole adsorbent resin organic matter residues in a desmodium styracifolium general flavone extractive with the headspace gas chromatography. The method is characterized in that a gaschromatograph allocated with an FID detecting instrument and a headspace sampling device are used; the chromatographic conditions are that a DB-1701 chromatographic column is adopted, the column flow rate ranges from 0.95 ml / min to 1.05 ml / min, the column temperature of the chromatographic column is characterized in that the initial temperature is 35 DEG C and is kept for 4 min, then the temperature rises with the rate ranging from 9 DEG C / min to 11 DEG C / min until the temperature is 90 DEG C, and finally the temperature rises with the rate ranging from 19 DEG C / min to 21 DEG C / min until the temperature is 230 DEG C; the temperature of the FID detecting instrument is 250 DEG C; the headspace parameters are that the holding temperature of a headspace bottle ranges from 138 DEG C to 142 DEG C, and the holding time of the headspace bottle ranges from 28 min to 32 min. The large-hole adsorbent resin organic matter residues are selected from at least one of normal hexane, benzene, toluene, dimethylbenzene, styrene and divinylbenzene. The method is simple, convenient, rapid, high in sensitivity, good in accuracy, high in specificity and good in reproducibility, and can be effectively used for detecting the residual quantity of large-hole adsorbent resin organic matter in the desmodium styracifolium general flavone extractive.

Description

technical field [0001] The invention relates to the field of detection methods for drug impurities in new traditional Chinese medicine technology, in particular to a method for detecting organic matter residues in macroporous adsorption resins in Desmodium sativa total flavonoids extract by headspace gas chromatography. Background technique [0002] Desmodium spp. is a plant of the genus Fabaceae, and it is recorded as a commonly used medicinal material in the first part of the 2005 edition of the Pharmacopoeia of the People's Republic of China. At the same time, the prescription preparation "Shilintong Tablet" recorded in the Pharmacopoeia has only a single herb of Desmodium sativa, which is used to treat urinary tract infection, urinary stones, cholecystitis and other diseases. The extraction and preparation process of "Shilintong Tablet" is relatively simple, the effective part is not clear, and the level of quality control indicators needs to be improved. Desmodium styl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 王学海许勇李莉娥杨仲文冯芸杨成兵李荣臻杨婷余艳平黄璐
Owner WUHAN OPTICS VALLEY HUMANWELL BIO PHARMA
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