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HPLC-MS/MS (high performance liquid chromatography-tandem mass spectrum) method for detecting nitroimidazole residues in royal jelly

A high-performance liquid chromatography, nitroimidazole technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of difficulty in extracting nitroimidazole drugs, etc., to promote the extraction of protein precipitants, promote salting out, promote Extracted effects

Active Publication Date: 2018-07-20
杭州康力食品有限公司
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  • Description
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Problems solved by technology

[0004] However, when using HClO 4 During the process of precipitating protein, due to HClO 4 The protein precipitation produced by the addition of nitroimidazoles will wrap nitroimidazoles, making it difficult to extract nitroimidazoles, which needs to be improved

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  • HPLC-MS/MS (high performance liquid chromatography-tandem mass spectrum) method for detecting nitroimidazole residues in royal jelly
  • HPLC-MS/MS (high performance liquid chromatography-tandem mass spectrum) method for detecting nitroimidazole residues in royal jelly
  • HPLC-MS/MS (high performance liquid chromatography-tandem mass spectrum) method for detecting nitroimidazole residues in royal jelly

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Embodiment Construction

[0032] The present invention will be described in further detail below in conjunction with the accompanying drawings.

[0033] The proportioning table of table 1 embodiment 1-5

[0034]

[0035] The concrete steps of embodiment 1-5:

[0036] refer to figure 1 with 2 , a method for measuring nitroimidazole residues in royal jelly by high performance liquid chromatography tandem mass spectrometry, the raw materials used in the method include metronidazole, Metronidazole, CAS: [443-48-1], purity > 99.4%; Pyridazole, ronidazole, CAS: [7681-76-7], purity > 99.0%; Dimetridazole, dimetridazole, CAS: [551-92-8], purity > 98.5%; D3-Dimetridazole, Dimetridazole -d3, CAS: 64678-69-9, purity > 98%; ethyl acetate, acetonitrile, dichloromethane, chloroform, tetrachloromethane of pesticide residue grade; analytically pure sodium chloride, sodium hydroxide And potassium hydroxide; for superior grade pure n-hexane; for liquid chromatography pure acetonitrile, formic acid; water; mobile ...

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Abstract

The invention discloses an HPLC-MS / MS (high performance liquid chromatography-tandem mass spectrum) method for detecting nitroimidazole residues in royal jelly. The method comprises a procedure of royal jelly sample treatment, and the procedure of royal jelly sample treatment comprises the following steps: a temporary working solution of a dimetridazole deuterated internal standard is added to a royal jelly sample, and then an organic solvent is added for whirling and dissolving; then a protein precipitant is added for whirling and dissolving, and an upper inorganic layer is obtained through centrifugation; a pH regulator is added to the inorganic layer for regulating pH, then ethyl acetate is added for extraction, and an organic layer is obtained and blow-dried by nitrogen; then ultrasonic dissolving is performed with a mobile phase, n-hexane is added for whirling degreasing, a mobile phase layer is obtained through centrifugation and passes through a filter membrane, and a sample solution for machine detection is prepared, wherein one of the protein precipitant and the pH regulator is an acid, and the other is a base. The method has the beneficial effects that protein precipitates can be prevented from wrapping nitroimidazole drugs, and sensitivity of the method is further improved.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for detecting nitroimidazole residues in royal jelly by high performance liquid chromatography tandem mass spectrometry. Background technique [0002] Nitroimidazole drugs are veterinary drugs containing an imidazole ring connected to a nitro group at the fifth position in the molecule, and are often used to prevent and treat specific bacteria and protozoan diseases. Due to the potential carcinogenicity, teratogenicity, mutagenicity and genotoxicity of nitroimidazole compounds, EU countries, Japan and other countries stipulate that drug residues in animal-derived foods should not be detected, that is, below the detection limit of the detection method. Royal jelly is also a medicinal animal-derived food, but its complex matrix and difficult sample purification lead to low accuracy in the determination of nitroimidazoles in royal jelly. [0003] The Chinese patent with publication nu...

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 张暘
Owner 杭州康力食品有限公司
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