Abstract:A novel, simple and rapid method was established for the simultaneous determination of four veterinary drugs (neomycin, griseofulvin, polymyxin B, olaquindox and its metabolite 3-methyl-quinoxaline-2-carboxylic acid (MQCA)) in muscle tissues of food-producing animals by solid phase extraction (SPE) coupled with high performance liquid chromatography tandem triple quadrupole mass spectrometry (HPLC-MS-MS). After homogenized, muscle tissues were extracted with a mixture of acetonitrile and 5% formic acid solution and the extract was purified by an HLB solid phase extraction column, separated by HPLC, detected by positive electrospray ionization in multiple reaction monitoring mode (MRM), and quantified by an external standard method. Under the optimal conditions, the calibration for all five analytes showed a linear relationship in the range of 1.0–200.0 μg/L with correlation coefficients higher than 0.998 0 and the limit of detection was 5.0 μg/kg for neomycin, griseofulvin, polymyxin B and 0.5 μg/kg for olaquindox and MQCA, respectively. The mean recoveries of spiked samples (spiked concentration levels: 20.0, 40.0 and 200.0 μg/L for neomycin, griseofulvin and polymyxin B; 2.0, 4.0 and 20.0 μg/L for qlaquindox and its metabolite) were ranged from 82.1% to 98.4% with relative standard deviation (RSD, n = 6) between 2.2% and 6.7%. This method is accurate, simple, rapid and applicable to the detection of veterinary drugs in muscle tissues.
耿 宁,卢 剑. 高效液相色谱-串联质谱法测定肌肉组织中4种兽药残留[J]. 肉类研究, 2017, 31(8): 39-43.
GENG Ning, LU Jian. Simultaneous Determination of Four Veterinary Drugs in Edible Muscle Tissues by High Performance Liquid Chromatography-Ttandem Mass Spectrometry. Meat Research, 2017, 31(8): 39-43.