UPLC-MS/MS simultaneous flux detection method for multiclass veterinary drug residue in raw fresh milk

A detection method and technology for veterinary drug residues are applied in the detection field of veterinary drug residues, which can solve the problems of complex pretreatment, single type of veterinary drugs, and difficulty in quantification.

Inactive Publication Date: 2015-07-08
INST OF ANIMAL SCI OF CHINESE ACAD OF AGRI SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are technical problems in the existing detection methods, such as single type of veterinary drug, complicated pre-treatment, and difficult quantification. It is urgent to develop a simultaneous quantitative analysis method for multiple groups of veterinary drug residues.

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  • UPLC-MS/MS simultaneous flux detection method for multiclass veterinary drug residue in raw fresh milk
  • UPLC-MS/MS simultaneous flux detection method for multiclass veterinary drug residue in raw fresh milk
  • UPLC-MS/MS simultaneous flux detection method for multiclass veterinary drug residue in raw fresh milk

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] Example 1 Establishment of UPLC-MS / MS simultaneous throughput detection method for multiple groups of veterinary drug residues in fresh milk

[0088] 1. Experimental method

[0089] 1.1 Sample extraction and purification

[0090] Weigh 1g of milk sample, put it in a 10mL centrifuge tube, add 0.5mL of water and 3mL of acetonitrile, vortex for 5min, centrifuge at 10000r / min for 10min, take the supernatant in another 10mL centrifuge tube, blow nitrogen to 1mL, add 3mL NaH 2 PO 4 solution, adjust the pH to 8.5, and vortex for 5 minutes.

[0091] Sequentially use 2mL methanol, 2mL water, 2mL NaH 2 PO 4 (pH 8.5) solution to pre-activate the HLB solid-phase extraction column; after taking all the extracts through the column, successively use 2mL NaH 2 PO 4 (pH 8.5) solution, 1 mL of water, and finally eluted with 3 mL of 1:1 acetonitrile / water solution and 1 mL of acetonitrile. The collected solution was blown with nitrogen gas at 40°C until the volume was less than 1....

experiment example 1

[0108] Experimental example 1 Methodological validation of UPLC-MS / MS simultaneous throughput detection method for multiple groups of veterinary drug residues in fresh milk

[0109] According to the "NY / T 1896-2010 Laboratory Quality Control Specifications for Veterinary Drug Residues" issued by the Ministry of Agriculture of China, the European Commission's 2002 / 657 / EC "On Evaluation of Analytical Methods and Interpretation of Results in European Commission Resolution 96 / 23 / EC" and FDA's "About The Guidelines for Bioanalytical Procedures require that veterinary drug residue analysis methods need to be quality controlled and validated through limits of detection (LOD), limits of quantitation (LOQ), standard curves, recovery rates, and precision.

[0110] 1. Linear range and detection limit

[0111] Add different concentrations of mixed standard working solutions to the blank milk sample. According to the corresponding value and sensitivity of the instrument, the concentrations...

experiment example 2

[0135] Experimental Example 2 Sample Extraction and Optimization of Purification Conditions

[0136] 1. Optimization of sample extraction conditions

[0137] The main purpose of sample extraction is to remove milk protein and milk fat, and to dissolve the veterinary drug analytes in the sample to the greatest extent. According to the UPLC-MS / MS simultaneous flux detection method of multiple groups of veterinary drug residues established in Example 1, under the condition of other test conditions unchanged, the following three schemes were tested for sample extraction respectively:

[0138] A: 1mL of milk is directly diluted with 3mL of water, centrifuged at 10000r, and passed through the HLB column.

[0139] B: Dilute 1mL milk with 0.5mL water, add 3mL acetonitrile to precipitate protein, centrifuge at 10000r, pass through HLB column (equivalent to water: acetonitrile = 1:2).

[0140] C: Add 4mL acetonitrile directly to 1mL milk to precipitate protein, centrifuge at 10000r, a...

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Abstract

The invention discloses a UPLC-MS / MS simultaneous flux detection method for multiclass veterinary drug residue in raw fresh milk. The method includes the steps of: (1) extracting a veterinary drug compound in a to-be-detected sample to obtain an extracted solution; (2) concentrating the extracted solution, and then regulating the pH to 7.5-10.0 to obtain a column passing solution; (3) activating a solid phase extraction column; and (4) loading the column passing solution on the activated solid phase extraction column, leaching the solid phase extraction column with leacheate, then conducting elution with eluent, collecting the eluent, carrying out concentration, redissolving and filtration by a filter membrane, then performing qualitative and quantitative determination by UPLC-MS / MS. The method provided by the invention can simultaneously detect 38 veterinary drug residue in raw fresh milk, and has the characteristics of high sensitivity and low detection limit. The matrix standard curve correlation degree, the standard addition recovery rate of the method and the intra-day and inter-day precision are all accord with the China, European Union and international veterinary drug residue analysis method requirements. The method provided by the invention provides efficient and accurate detection means for raw fresh milk veterinary drug residue risk analysis and warning research.

Description

technical field [0001] The invention relates to a detection method for veterinary drug residues, in particular to a UPLC-MS / MS simultaneous throughput detection method for multiple groups of veterinary drug residues in fresh milk, and belongs to the technical field of detection of veterinary drug residues. Background technique [0002] Residues of veterinary drugs in raw milk directly affect human health. Although ELISA and Delvo kits are commonly used at present, although they have the advantages of being fast, convenient, and easy to implement, they can only determine whether there are veterinary drug residues in raw milk and whether the residues are However, it is difficult to determine the actual ingredients and content in raw milk. [0003] Ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS / MS) is a quantitative analysis method that uses mass spectrometry detector as the main identification method and integrates the separation process of high perf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 郑楠韩荣伟于忠娜张养东李松励王军屈雪寅王加启
Owner INST OF ANIMAL SCI OF CHINESE ACAD OF AGRI SCI
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