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UPLC-MS/MS method for analyzing four categories and 29 types of restricted veterinary drug residues in animal foodstuff

A technology for animal food and veterinary drug residues, applied in the direction of analysis of materials, material separation, measurement devices, etc., can solve the problems of special physical and chemical properties, high detection costs, difficult simultaneous extraction and purification of veterinary drugs, etc. Good performance and low cost

Inactive Publication Date: 2016-02-10
TIANJIN INSTITUE OF QUALITY STANDARD & TESTING OF AGRICULTUAL PRODS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the special physical and chemical properties of tetracycline veterinary drugs, it is difficult to extract and purify simultaneously with other veterinary drugs. Therefore, there are no literature reports on the simultaneous detection of tetracyclines and sulfonamides, quinolones, amantadine and other veterinary drugs.
In addition, most of the reported methods use solid-phase extraction column purification, and the detection cost is also high.

Method used

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  • UPLC-MS/MS method for analyzing four categories and 29 types of restricted veterinary drug residues in animal foodstuff
  • UPLC-MS/MS method for analyzing four categories and 29 types of restricted veterinary drug residues in animal foodstuff
  • UPLC-MS/MS method for analyzing four categories and 29 types of restricted veterinary drug residues in animal foodstuff

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take the chicken sample A to be tested as the sample, adopt the method of the present invention for sample pretreatment, and adopt ultra-high performance liquid chromatography-tandem mass spectrometry for determination. The preparation method is as follows:

[0040] 1. Instruments and reagents:

[0041] United States WatersAcquity TM UPLC ultra-high performance liquid chromatograph, QuattroPremierXE triple quadrupole mass spectrometer; Swiss Mettler electronic balance (sensitivity 0.00001g); vortex mixer; desktop high-speed centrifuge; American Milli-Q ultrapure water meter.

[0042] 29 kinds of veterinary drug standards, the purity is not less than 99%; acetonitrile and formic acid are chromatographically pure, n-hexane, anhydrous sodium sulfate are analytically pure, water is ultra-pure water; adsorbent C18, NH2, specifications 40-60 mesh .

[0043] 2. Sample preparation method:

[0044] Accurately weigh 2.00g (accurate to 0.01g) of the homogenized chicken sample into a 50mL...

Embodiment 2

[0054] As described in Example 1, the test chicken liver sample B was measured, and the measured residual amounts of 29 target veterinary drugs in sample B are shown in Table 5.

Embodiment 3

[0056] As described in Example 1, the test pork sample C was measured, and the measured residues of 29 target veterinary drugs in sample C are shown in Table 5.

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Abstract

The invention provides an UPLC-MS / MS method for analyzing four categories and 29 types of restricted veterinary drug residues in animal foodstuff. The method is characterized in that an advanced QuEChERS method is adopted for conducting sample preprocessing, a sample is subjected to McIlvaine buffering liquid-acetonitrile extraction, an extracting solution is subjected to acidification and salting out, a small amount of acetonitrile phase is taken, a C18 and NH2 adsorbing agent is utilized for conducting dispersive solid-phase extraction and purification, after purification liquid is subjected to concentration and volume setting, an ultra-high performance liquid chromatography-tandem mass spectrometer (UPLC-MS / MS) is adopted to conduct detection. The problem that it is difficult for tetracycline class veterinary drug to be extracted and purified along with other types of veterinary drugs is solved, meanwhile the sample processing steps are simplified, the UPLC-MS / MS method has the advantages of being efficient, rapid, low in cost, simple and convenient to operate, good in purification effect and high in sensitivity, and the accuracy and precision both meet the requirement of a multi-residue analysis method.

Description

Technical field: [0001] The invention belongs to the technical field of determination of veterinary drug residues in animal foods, and relates to whether 29 kinds of restricted veterinary drug residues in chicken, chicken liver, pork and pig liver samples total 29 kinds of restricted veterinary drugs in four categories: tetracyclines, amantadine, sulfonamides and quinolones. The measurement method, in particular, adopts the modified QuEChERS method as the pre-measurement processing method. Background technique: [0002] Veterinary drug residues refer to the original form of the drug, metabolites and drug impurities accumulated or stored in animal cells, tissues or organs after the drug is administered to animals. Veterinary drug residues are mainly caused by unreasonable use of drugs to treat animal diseases and as feed additives. Although my country has formulated the "Maximum Residue Limits of Veterinary Drugs in Animal Foods" and the "Regulations for the Use of Feed Drug Addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李娜张玉婷刘磊邵辉李辉李晶宋淑荣郭永泽
Owner TIANJIN INSTITUE OF QUALITY STANDARD & TESTING OF AGRICULTUAL PRODS
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