Detection method for simultaneously measuring residue of nitroimidazoles drugs in royal jelly

A technology for nitroimidazoles and a detection method is applied in the detection field of simultaneous determination of the residues of multiple nitroimidazoles in royal jelly, and achieves the effects of high sensitivity, accurate results and elimination of sample matrix effects.

Inactive Publication Date: 2009-11-04
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0007] In order to solve the difficult problem of the detection of nitroimidazole drug residues in royal jelly, the object of the present invention is to provide a liquid chromatography-mass spectrometry / mass spectrometry method with strong specificity, high sensitivity and accurate detection of nitroimidazole drug residues in royal jelly. detection method

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  • Detection method for simultaneously measuring residue of nitroimidazoles drugs in royal jelly
  • Detection method for simultaneously measuring residue of nitroimidazoles drugs in royal jelly
  • Detection method for simultaneously measuring residue of nitroimidazoles drugs in royal jelly

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Embodiment Construction

[0037] A detailed description will be given below of specific embodiments of the present invention.

[0038]The detection method for simultaneously measuring multiple nitroimidazoles drug residues in royal jelly of the present invention comprises the following steps:

[0039] 1. Extraction

[0040] Weigh 2g of the sample (accurate to 0.01g) and place it in a 50mL centrifuge tube with stopper, add 0.2mL dimetidazole-d3, ronidazole-d3 isotope internal standard solution (200ng / mL), hydroxydimethylnitrate Imidazole-d3, Hydroxypronidazole-d3, Pronidazole-d3 isotope internal standard solution (100ng / mL), add 10mL water, mix well, let stand for 2min, then add methanol to 20mL, put on a vortex mixer Mix at 2000r / min for 1min, centrifuge at 6000r / min for 10min, filter, pipette 10.0mL supernatant, add 10mL phosphate buffer solution (dissolve 13.8g sodium dihydrogen phosphate in 950mL water, oxidize with 0.1mol / L hydroxide Adjust the pH value of the solution to 8.0 with sodium solution...

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Abstract

The invention relates to a method for measuring the residue of nitroimidazoles drugs in royal jelly, in particular to a method for measuring the residue of nitroimidazoles drugs, such as 1-(2-hydroxyethyl)-2-hydroxy-methyl-5-nitroimidazol (MNZOH), 2-methyl-5-nitroimidazole, 2-hydroxymethyl-1-methyl-5-nitroimidazole (DMZOH / HMMNI), metronidazole (MNZ), dimetridazole (DMZ), ronidazole (RNZ), 5-chloro-1-methyl-4-nitroimidazole, 5-nitrobenzimidazole, 2-(2'-hydroxyisopropyl)-1-methyl-5-nitroimidazol (IPZOH), 2-isopropyl-1-methyl-5-nitroimidazol (Ipronidazole, IPZ) and the like, in the royal jelly by the liquid chromatography-mass spectrometry / mass spectrometer (LC-MS / MS). The method comprises the following steps: precipitating protein by methanol; extracting; further carrying out the purification using HLB (hydrophilic-lipophilic balance) and C18 solid-phase extraction (SPE) columns; and measuring the residue by LC-MS / MS. The invention has the characteristics of high specificity, high sensitivity and accurate results, and allows for the measurement of both the nitroimidazoles original drugs and the metabolites thereof; the lower limit of detection (10 mug / kg) in the method meets the existing requirements for the residue of nitroimidazoles drugs in the royal jelly at home and aboard; the recovery rate ranges from 70.7% to 105.0%; and the relative standard deviation (RSD) is lower than 12.7%.

Description

technical field [0001] The invention relates to a method for the residual amount of nitroimidazoles in royal jelly, in particular to the determination of hydroxymetronidazole, 2-metronidazole, hydroxydimethylnidazole, metronidazole, Method for residues of nitroimidazoles such as dimetidazole, ronidazole, clometrazole, benzidazole, hydroxypronidazole and pronidazole. Background technique [0002] Nitroimidazoles are a class of antibiotics and antiprotozoal drugs, which are mainly used for the treatment and prevention of poultry histoflagellates (turkey blackhead disease), bovine trichomoniasis and porcine treponema dysentery and effective medicine for parasites in fish. Their common feature is that the imidazole ring has N-1 methyl and 5-nitro substituents, and only the substituent at the C-2 position is different. Nitroimidazole drugs are rapidly metabolized, and the main metabolite is that the methyl group on the C2 of the imidazole ring is oxidized to a hydroxymethyl gro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06B01D15/08
Inventor 谢文陈笑梅丁慧瑛奚君阳钱艳
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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