Method for detecting drugs in goat milk and goat milk products

A detection method and drug technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of small quantity and types of prohibited and restricted drugs in detection

Inactive Publication Date: 2018-01-09
CHINA ANIMAL DISEASE CONTROL CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention aims at the problem that the number of prohibited and restricted drugs detected in the prior art is small and the types are few, and establishes a system covering β-receptor agonists (27 types), quinolones (20 types), macrolides (3 types), Ultra-high performance liquid chromatography-mass spectrometry for 7 categories of 59 veterinary drugs, including benzimidazoles (3 types), sedatives (2 types), antivirals (2 types) and pleuromutilins (2 types); For samples such as goat milk and its products, it makes up for the lack of comprehensiveness of existing detection methods and standards

Method used

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  • Method for detecting drugs in goat milk and goat milk products
  • Method for detecting drugs in goat milk and goat milk products
  • Method for detecting drugs in goat milk and goat milk products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0137] 1 Instruments and materials

[0138] 1.1 Instrument

[0139] Ultra-high performance liquid chromatography (H-Class UPLC, Waters company); triple quadrupole mass spectrometer (xevo TQ-XS, Waters company); MassLynx v 4.1 data processing software (Waters company); 3K15 centrifuge (Sigma company ); Milli-Q pure water instrument (millipore company); Nitrogen blowing instrument (Organomation company).

[0140] 1.2 Materials

[0141] Organic solvents such as methanol, acetonitrile, and formic acid were chromatographically pure (Fisher); SPE column (60mg, 3cc, waters); chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm, waters).

[0142] β-receptor agonists, quinolones, macrolides, benzimidazoles, sedatives, antivirals and pleuromutilins, etc. 7 categories of 59 kinds of veterinary drugs were purchased from Dr. More than 97%.

[0143] Goat milk and milk powder samples were purchased from e-commerce supermarkets, and the negative samples confirmed by LC-MS / MS a...

Embodiment 2

[0180] 20.0 μL of the 27 kinds of β-receptor agonist drug mixture (concentration: 500 ng / ml) was added to 2 g blank negative goat milk sample. Add 10mL 0.5% formic acid acetonitrile, vortex mix for 5min, 9500r·min -1 Centrifuge for 5 minutes, take the supernatant in a 50mL centrifuge tube, repeat the extraction once, combine the extracts, and pass through the purification column.

[0181] Purification: transfer all the extracts to the SPE column activated with 85% acetonitrile water in advance, keep the flow rate 1d s -1 , collect all the filtrate, blow it with nitrogen gas at 40°C until it is nearly dry, use the initial mobile phase to adjust the volume to 1 mL, 9500r·min -1 Centrifuge for 5 minutes, and filter the upper liquid layer with a 0.22 μm filter membrane, and wait for determination on the machine.

[0182] Chromatographic conditions

[0183] Chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm); flow rate: 0.3mL min -1 ;Column temperature: 35°C; Mobi...

Embodiment 3

[0187] 20.0 μL of the 20 kinds of quinolone drug mixture (concentration: 500 ng / ml) was added to 2 g blank negative goat milk sample. Add 10mL 0.5% formic acid acetonitrile, vortex mix for 5min, 9500r·min -1 Centrifuge for 5 minutes, take the supernatant in a 50mL centrifuge tube, repeat the extraction once, combine the extracts, and pass through the purification column.

[0188] Purification: transfer all the extracts to the SPE column activated with 85% acetonitrile water in advance, keep the flow rate 1d s -1 , collect all the filtrate, blow it with nitrogen gas at 40°C until it is nearly dry, use the initial mobile phase to adjust the volume to 1 mL, 9500r·min -1 Centrifuge for 5 minutes, and filter the upper liquid layer with a 0.22 μm filter membrane, and wait for determination on the machine.

[0189] Chromatographic conditions

[0190] Chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm); flow rate: 0.3mL min -1 ;Column temperature: 35°C; Mobile phase ...

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Abstract

The invention provides a method for detecting 7 classes of 59 forbidden drugs in goat milk and goat milk products. The method comprises the following steps: (1) sample pretreatment: extracting a to-be-detected sample with an acid organic solvent, carrying out purification by virtue of an SPE column, dissolving a purified liquid by virtue of a primary flow phase, and carrying out UPLC-MS/MS detection; and (2) detection of 59 to-be-detected forbidden drugs: detecting the pretreated sample by virtue of an ultra-high performance liquid chromatography-mass spectrometry under specified instrument conditions of the method. The method has the advantages that many drugs can be detected, the type of the drugs is rich, the detection time is short, the sensitivity is high, and a result is accurate andstable; and meanwhile, the detection blank that multiple types and quantity of drugs in the goat milk and the goat milk products can be simultaneously detected is filled up, and the method has important significances to the guarantee of the body health of consumers and the increase of export trade competitiveness of the goat milk and the goat milk products.

Description

technical field [0001] The invention relates to a method for detecting prohibited and restricted drugs, in particular to a method for detecting 59 kinds of prohibited and restricted drugs in 7 categories in goat milk and its products. Background technique [0002] Milk and dairy products are an indispensable part of consumers' dietary composition, and their nutritional composition, quality and safety have received more and more attention. Among them, milk sources have gradually expanded from cow milk to goat milk and its products. , has the characteristics of small fat particles and protein particles, rich minerals and vitamins, and is easier to be absorbed by the human body; and goat milk is closer to human milk in terms of basic structure and nutritional ratio, and is especially suitable for infants and young children. At the same time, аS in goat milk -The content of foreign protein such as casein is less, which can greatly reduce the occurrence of allergic reactions. Wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 刘洪斌蔡英华李颖田亚平姜艳彬于雷
Owner CHINA ANIMAL DISEASE CONTROL CENT
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