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
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Metaphosphoric acid-Methanol Acetic acid Acetonitrile
Solid Phase Extraction Column Chromatography Column
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)