Experimental determination of macrolide antibiotic residues in fish and meat

Summary

Macrolide antibiotics are antibiotics commonly used as veterinary drugs. There are many methods available for the determination of macrolide residues in animal tissues. Source: Food Safety Monitoring Technology (Chemical Industry Press)

Operation method

HPLC-ESI-MS-SIM method

Materials and Instruments

Fish Chicken
Metaphosphoric acid-Methanol Acetic acid Acetonitrile
Solid Phase Extraction Column Chromatography Column

Move

1. Extraction and purification

Weigh 5 g of sample, 100 mL of 0.2% metaphosphoric acid-methanol (6 + 4), high-speed homogenization for 2 min, filtration, filtrate at 40 ℃ under reduced pressure and concentrated to a volume of about 25 mL, poured into 60 mg HLB solid-phase extraction column (pre-activated with 5 mL of methanol and 10 mL of water) 10 mL of water elution, 5 mL of methanol elution. The eluate was concentrated to dryness at 40 ℃ under reduced pressure, dissolved in l mL of 30% methanol solution, and 50 L of the eluate was injected into the sample for analysis.

2. Chromatography and mass spectrometry conditions

Chromatographic column: TSK-gelSuperODS (100 mm×2 mm) with gradient elution (0 min, 85% 0.2% acetic acid, 15% acetonitrile containing 0.2% acetic acid, 20 min-25 min, 50% 0.2% acetic acid, 50% acetonitrile containing 0.2% acetic acid)
Flow rate: 0.2 mL/ min
Column temperature: 40 ℃
ESI: (+)
Atomizing gas: (N2, 40 psi)
Dry Gas: (N2, 10 L/min, 350 °C)
Cone Voltage: (4500 V)

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