A method for detecting drugs in goat milk and its products

A detection method and product technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of few types, detection of prohibited and restricted drugs, etc.

Inactive Publication Date: 2021-01-26
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 small, and establishes a system covering β-receptor agonists (27 types), sulfonamides (15 types), quinolones (20 types), and macrocyclic endogenous drugs. Ultra performance liquid chromatography-mass spectrometry of 74 kinds of veterinary drugs in 8 categories including esters (3 kinds), benzimidazoles (3 kinds), sedatives (2 kinds), antivirals (2 kinds) and pleuromutilins (2 kinds) usage; in addition, the established method makes up for the lack of comprehensiveness of existing detection methods and standards for samples such as goat milk and its products

Method used

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  • A method for detecting drugs in goat milk and its products
  • A method for detecting drugs in goat milk and its products
  • A method for detecting drugs in goat milk and its products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0136] 1 Instruments and materials

[0137] 1.1 Instrument

[0138] 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).

[0139] 1.2 Materials

[0140] 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).

[0141] β-receptor agonists, sulfonamides, quinolones, macrolides, benzimidazoles, sedatives, antivirals and pleuromutilins and other 8 categories of 74 kinds of veterinary drugs were purchased from Dr. Ehrenstorfer and Braunwell in Germany. All above 97%.

[0142] Goat milk and milk powder samples were purchased from e-commerce super...

Embodiment 2

[0179] 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.

[0180] Purification: Transfer all the extract to an SPE column activated with 85% acetonitrile water in advance, keep the flow rate at 1 drop per second, collect all the filtrate, blow it to nearly dry with nitrogen at 40°C, and dilute to 1mL with the initial mobile phase, 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.

[0181] Chromatographic conditions

[0182] Chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm); flow rate: 0.3mL min -1 ;Column temperature: 35°C; Mobile phase A: m...

Embodiment 3

[0186] 20.0 μL of the 15 kinds of sulfonamide 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.

[0187] Purification: Transfer all the extract to an SPE column activated with 85% acetonitrile water in advance, keep the flow rate at 1 drop per second, collect all the filtrate, blow it to nearly dry with nitrogen at 40°C, and dilute to 1mL with the initial mobile phase, 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.

[0188] Chromatographic conditions

[0189] Chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm); flow rate: 0.3mL min -1;Column temperature: 35°C; Mobile phase A: methanol,...

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Abstract

The invention provides a method for detecting 8 categories of restricted drugs in goat milk and products thereof, wherein the number of the restricted drugs is 74. The method comprises: (1) pre-treating a sample: extracting a sample to be detected with an acid organic solvent, purifying with a SPE column, and dissolving the purified liquid by using an initial mobile phase so as to be used for detection with UPLC-MS / MS; and (2) determining 74 restricted drugs: determining the pre-treated sample by using ultra performance liquid chromatography-LC-MS under the instrument condition specified by the method. According to the present invention, the method has advantages of more types of detected drugs, rich variety, short detection time, high sensitivity and accurate and stable results, can makesup for the absence of the simultaneous detection of multiple drugs in goat milk and dairy products, and provides the important significance for the assurance of the health body of consumers and the improvement of the export competitiveness of goat milk and dairy products.

Description

technical field [0001] The invention relates to a method for detecting prohibited and restricted drugs, in particular to a method for detecting 74 kinds of prohibited and restricted drugs in 8 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 Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
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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