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为建立同时检测牛奶中青霉素G及青霉噻唑酸的UPLC-MS/MS检测法,将牛奶样品经乙腈∶乙醇(3∶1,V∶V)提取后离心分离,用Oasis HLB固相萃取柱净化,进行超高效液相色谱-串联质谱法检测。青霉素和青霉噻唑酸在线性范围内相关系数在0.993以上,方法的检出限(LOD,S/N=3)为0.3μg/kg~0.5μg/kg,定量限(S/N=10)为1.0μg/kg~2.0μg/kg。选用基质添加标准曲线消除基质干扰,样品加标回收率为75.88%~106.01%,变异系数为6.65%~14.17%。说明方法的灵敏度高,重复性良好,为快速准确的检测该类药物提供可靠的技术支撑。
In order to establish UPLC-MS / MS method for the simultaneous determination of penicillin G and penicillin in milk, the milk samples were extracted by acetonitrile: ethanol (3: 1, V: V), centrifuged, Purification, ultra-high performance liquid chromatography - tandem mass spectrometry. The linear range of penicillin and penicillin was 0.993 and the detection limit (LOD, S / N = 3) was 0.3μg / kg ~ 0.5μg / kg with the limit of quantification (S / N = 10) 1.0 μg / kg to 2.0 μg / kg. Substrate add standard curve to eliminate matrix interference, sample spike recovery was 75.88% ~ 106.01%, coefficient of variation of 6.65% ~ 14.17%. Indicating that the method of high sensitivity, good reproducibility, rapid and accurate detection of such drugs provide a reliable technical support.