超高效液相色谱-串联质谱法对动物源性食品中13种β-内酰胺类药物残留的检测

Determination of 13 β-Lactam Residues in Food of Animal Origin by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了动物源性食品中青霉素G、青霉素V、阿莫西林、羧苄西林、氨苄西林、苯唑西林、氯唑西林、萘夫西林、头孢喹肟、头孢氨苄、头孢拉定、头孢唑啉和头孢哌酮13种β-内酰胺类药物残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经水和乙腈提取后,用正己烷去除脂肪,再用C18固相萃取柱净化,浓缩后用BEHC18色谱柱(50mm×2.1mm,1.7μm)分离,以0.1%甲酸乙腈溶液和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测。结果表明:在5～500μg/L的基质匹配标准溶液内13种β-内酰胺类药物均有良好的线性关系,相关系数(r)均大于0.998;样品中13种β-内酰胺类药物的检出限(LOD)均为1ng/g,定量下限(LOQ)均为2ng/g;在5～50ng/g的加标范围内13种β-内酰胺类药物的平均回收率为79%～99%,相对标准偏差(RSD)小于13.5%。

An ultra performance liquid chromatography - tandem mass spectrometry （UPLC - MS/ MS） method was established for the determination of penicillin G, penicillin V, amoxieillin, ear- benicillin, ampicillin, oxacillin, cloxacillin, nafcillin, eefquinome, cefalexin, eefradine, cefazo- lin and eefoperazone residues in food of animal origin. Samples were extracted by water and aeetoni- trile. The fat was removed by hexane, and the other impurities were removed by C18 SPE cartridge. The separation of 13 fl-laetams was performed on Waters Aequity UPLC BEH Cl8 column （50 mmx 2. 1 mm, 1.7 μm） using acetonitrile（0. 1% formic acid） -water（0. 1% formic acid）as gradient elution at a flow rate of 0.3 mL/min. The electrospray was operated in the positive ionization mode and 13 β-lac- tams were identified under multiple reaction monitoring（MRM） mode. The method was quantified by matrix-matched standard curves. Results showed that the calibration curves for 13 β-lactams had good linearity between the peak areas and the concentrations of 5 -500 μg/L, and the correlation coeffi- cients（r） were more than 0. 998. The detection limits for 13 β-laetams was 1 ng/g, and the quantifi- cation limits was 2 ng/g. The average recoveries at the spiked concentrations of 5 - 50 ng/g ranged from 79% -99% with RSDs less than 13.5% .