Method for detecting drugs in goat milk and products thereof
A detection method and drug technology, which can be applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of few types and small number of prohibited and restricted drugs in detection.
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Embodiment 1
[0140] 1 Instruments and materials
[0141] 1.1 Instrument
[0142] 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).
[0143] 1.2 Materials
[0144] 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).
[0145] 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%.
[0146] Goat milk and milk powder samples were purchased from e-commerce super...
Embodiment 2
[0182] 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.
[0183] 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.
[0184] Chromatographic conditions
[0185] Chromatographic column: Acquity UPLC BEH C18 (100mm×2.1mm, 1.7μm); flow rate: 0.3mL min -1 ;Column temperature: 35°C; Mobi...
Embodiment 3
[0189]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.
[0190] 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.
[0191] Chromatographic conditions
[0192] 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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