Detection method of nitrofuran drug metabolites in meat product

A detection method and nitrofuran technology are applied in measurement devices, instruments, scientific instruments and other directions, which can solve the problems of complex reagents and detection of nitrofuran metabolites, and achieve the effects of convenient pretreatment and simple reagents and reaction conditions.

A detection method and nitrofuran technology are applied in measurement devices, instruments, scientific instruments and other directions, which can solve the problems of complex reagents and detection of nitrofuran metabolites, and achieve the effects of convenient pretreatment and simple reagents and reaction conditions.

CN104297384AInactive Publication Date: 2015-01-21北京华都肉鸡公司
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  • Detection method of nitrofuran drug metabolites in meat product
  • Detection method of nitrofuran drug metabolites in meat product

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Pretreatment

[0032] Weigh 2g of a homogeneous sample (pork) in a centrifuge tube with a cover; add 10ml of methanol / water solution (methanol content 70%), mix well, centrifuge, discard the supernatant, and leave the solid residue of the sample for the next step use.

[0033] (2) Derivatization treatment

[0034] Add 2-nitrobenzaldehyde dimethyl sulfoxide solution (concentration in the extract is 0.1mmol / L) and hydrochloric acid solution (concentration in the extract is 0.1-0.2mol / L) in the sample solid residue extract , that is, the pH is about 0.9-1.1), then fill with nitrogen, and seal the cap of the centrifuge tube in a nitrogen environment (this can be airtight and dark, preventing the derivatives of 2-nitrobenzaldehyde and nitrofuran metabolites from be oxidized to improve derivatization efficiency); derivatize in a water bath at 90-99°C or an air bath at 90-104°C for 30-60 minutes; cool the hydrolysis derivative solution to below 15°C; adjust the pH value ...

Embodiment 2

[0039] (1) Pretreatment

[0040] Weigh 2 g of a homogeneous sample (chicken liver) in a centrifuge tube with a cover; add 20 ml of methanol / water solution (methanol content 50%), mix well, centrifuge, discard the supernatant, and save the solid residue of the sample for the next step For processing.

[0041] (2) Derivatization treatment

[0042] Add 2-nitrobenzaldehyde dimethyl sulfoxide solution (concentration in the extract is 0.1mmol / L) and hydrochloric acid solution (concentration in the extract is 0.1-0.2mol / L) in the sample solid residue extract , that is, the pH is about 0.9-1.1), then fill with nitrogen, and seal the cap of the centrifuge tube in a nitrogen environment (this can be airtight and dark, preventing the derivatives of 2-nitrobenzaldehyde and nitrofuran metabolites from be oxidized to improve the derivatization efficiency); derivatize in a 99°C water bath for 60 minutes; cool the hydrolysis derivative solution to 4°C; adjust the pH value of the hydrolysis ...

Embodiment 3

[0047] (1) Pretreatment

[0048] Weigh 2g of a homogeneous sample (egg) in a centrifuge tube with a cover; add 10ml of methanol / water solution (methanol content 90%), mix well, centrifuge, discard the supernatant, and leave the solid residue of the sample for the next step use.

[0049] (2) Derivatization treatment

[0050] Add 2-nitrobenzaldehyde dimethyl sulfoxide solution (concentration in the extract is 0.1mmol / L) and hydrochloric acid solution (concentration in the extract is 0.1-0.2mol / L) in the sample solid residue extract , that is, the pH is about 0.9-1.1), then fill with nitrogen, and seal the cap of the centrifuge tube in a nitrogen environment (this can be airtight and dark, preventing the derivatives of 2-nitrobenzaldehyde and nitrofuran metabolites from be oxidized to improve the derivatization efficiency); derivatize in an air bath at 90-104°C for 30 minutes; cool the hydrolysis derivative solution to 1°C; adjust the pH value of the hydrolysis derivative solut...

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Abstract

The application provides a detection method of nitrofuran drug metabolites in a meat product. The detection method comprises the following steps: (1) pretreatment comprising putting a sample into a pretreatment liquid, oscillating, then carrying out centrifugal separation, removing the clear liquid, and thus obtaining a solid residue; and (2) solid residue treatment comprising adding a derivatization agent into a sample solid residue extract liquid, carrying out derivatization treatment under conditions of heating, acidity and inert gas protection, after the derivatization treatment is completed, cooling, adjusting the pH to neutral, then centrifuging, taking the supernatant, then allowing the supernatant to pass through a solid-phase extraction column, leaching with a leaching liquid, carrying out elution treatment with an eluant to obtain an eluate, concentrating and drying the eluate, re-dissolving with a re-dissolving liquid, and thus obtaining a sample solution. The detection method can be applied to various animal-derived samples, and can shorten the hydrolyzed derivatization process to 30-60 minutes and shorten the whole detection process to 60-120 minutes.

Description

technical field [0001] The invention relates to a monitoring method for detecting drug residues, in particular to a method for detecting nitrofuran drug metabolites in meat products. Background technique [0002] At present, the Ministry of Agriculture Announcement No. 193 clearly stipulates that nitrofuran drugs are strictly prohibited from being used in food animals, but because of their obvious curative effect in treating intestinal bacterial infections and low prices, they are still illegally used in livestock and poultry breeding. Nitrofuran drug residues mainly detect its metabolites: 3-amino-2-oxazolidinone (AOZ), 5-methylmorpholine-3-amino-2-oxazolidinone (AMOZ), semicarbazide ( SEM), 1-aminohydantoin (AHD). Most of the nitrofuran metabolites are tightly bound to the protein, and only a small part exists in the free state, and its hydrolytic derivatization is the key link in the detection. [0003] At present, the representative methods for detecting residues of me...

Claims

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Application Information

Patent Timeline
21 Jan 2015
Publication
CN104297384A
IPC
G01N30/06
Inventors
郭黎明; 王宏卫