Simultaneous determination of amoxicillin and prednisolone in bovine milk using ultra-high performance liquid chromatography tandem mass spectrometry.
A rapid and sensitive ultra-high performance liquid chromatography tandem mass spectrometric method was developed for simultaneous quantification of amoxicillin and prednisolone in bovine milk. In this method, amoxicillin, prednisolone and the internal standards penicillin G-d(7) (for amoxicillin) and prednisolone-d(6) were extracted from bovine milk using acetonitrile. The C(18) solid phase extraction cartridges were selected for cleaning-up the extracts. The analytes were determined using a triple quadrupole mass spectrometry in positive electrospray ionization and multiple reaction monitoring mode. Calibration curves were linear over a concentration range of 2-1000 μg/kg for the analytes. The mean recoveries were 89.2-92.3% for amoxicillin and 98.7-102.3% for prednisolone. Limits of detection were 0.5 μg/kg for the analytes, and the limits of quantitation were 2 μg/kg. Decision limit (CCα) and detection capability (CCβ) have also been estimated for each analyte. The method was validated according to the Commission Decision 2002/657/EC and successfully applied to the analysis of amoxicillin and prednisolone in real samples.
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Hui
H
Li
Xi
X
Xia
Yanan
Y
Xue
Shusheng
S
Tang
Xilong
X
Xiao
Jiancheng
J
Li
Jianzhong
J
Shen
D000097:Acetonitriles; D000658:Amoxicillin / Q000032:analysis*; D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D008892:Milk / Q000737:chemistry*; D011239:Prednisolone / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*
D000097:Acetonitriles; D000658:Amoxicillin; D011239:Prednisolone; C032159:acetonitrile