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Method for determining residues of metabolites of four nitrofurans drugs in animal glue traditional Chinese medicine

A technology of nitrofuran and metabolites, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of eliminating matrix effects, high sensitivity, and optimizing operating back pressure

Inactive Publication Date: 2018-05-08
杭州市食品药品检验研究院
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Problems solved by technology

Traditional Chinese medicine glue is an important part of the traditional medicine treasure house of the motherland. It has a long history of use, rich sources of raw materials, complicated production processes, and extensive clinical applications. There is a large difference, and the detection of residues of nitrofuran drug metabolites in animal glue traditional Chinese medicine is very difficult

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  • Method for determining residues of metabolites of four nitrofurans drugs in animal glue traditional Chinese medicine
  • Method for determining residues of metabolites of four nitrofurans drugs in animal glue traditional Chinese medicine
  • Method for determining residues of metabolites of four nitrofurans drugs in animal glue traditional Chinese medicine

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Embodiment 1

[0076] Example 1: A method suitable for dispersive solid phase extraction combined with solid phase extraction purification-ultra-high performance liquid chromatography-tandem mass spectrometry for the residues of four nitrofuran drug metabolites in colloidal Chinese medicines, the following steps are performed in sequence:

[0077] 1), prepare the sample solution to be tested:

[0078] (1.1), take the gum class Chinese medicine as the sample to be tested, pulverize it into powder with a Chinese medicine pulverizer, and mix well;

[0079] (1.2) Weigh 2 g of the above-mentioned powder sample, accurate to 0.01 g, place it in a polyethylene centrifuge tube, add 10 ml of 0.2 mol / L hydrochloric acid solution, and ultrasonically dissolve;

[0080] (1.3) Add 100ul 0.5mg / ml pepsin to the dissolved sample solution, and simultaneously add 100ul 2-nitrobenzaldehyde solution (concentration of 2-nitrobenzaldehyde solution is 0.1mol / L, dissolved in ethanol), 37 ℃ shake in constant temperat...

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Abstract

The invention discloses a method for determining residues of metabolites of four nitrofurans drugs in an animal glue traditional Chinese medicine. The method comprises the following steps: preparing to-be-tested sample solution; preparing standard solution; injecting a standard series of working solution into a liquid chromatograph / mass spectrometer, determining appearance positions of the metabolites of the four nitrofurans drugs and qualitative and quantitative determination ion pairs thereof, and making a standard curve equation by taking the abundance of the quantitative ion pairs as a vertical coordinate and taking the concentration as a horizontal ordinate; substituting data obtained by corresponding detection for the to-be-tested sample solution into the standard curve equation forcalculation, so as to obtain the contents of the metabolites of all the nitrofurans drugs in the to-be-tested sample. The metabolites of the four nitrofurans drugs are: a furanzolidon metabolite (AOZ), a furaltadone metabolite (AOMZ), a furacilin metabolite (SEM) and a furadantin metabolite (AHD).

Description

technical field [0001] The invention relates to a dispersive solid-phase extraction combined with pass-through solid-phase extraction purification-ultra-high performance liquid chromatography-tandem mass spectrometry detection method suitable for four nitrofuran drug metabolite residues in animal glue traditional Chinese medicines. Background technique [0002] Nitrofuran drugs are a class of synthetic antibiotics with a 5-nitrofuran core structure, mainly including furazolidone (FZD), nitrofurantoin (NFT), nitrofurazone (NFZ), and furaltadone (FTD). [0003] Nitrofuran drugs have a broad-spectrum inhibitory and killing effect on bacteria, and have effects on a large number of Gram-positive and negative bacteria, fungi, and protozoa; Nitrofuran drugs have chronic toxicity and can cause gastrointestinal reactions, such as Nausea, vomiting, anorexia, diarrhea, etc. can also cause hemolytic anemia and jaundice; long-term or high-dose use of nitrofuran drugs can produce toxic ef...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 励炯贾彦博孙岚王红青林伟杰
Owner 杭州市食品药品检验研究院
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