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目的建立一种高效液相色谱-串联质谱联用技术测定乳制品中7种青霉素类抗生素(氯唑西林、萘夫西林、苯唑西林、青霉素V、阿莫西林、青霉素G、氨苄西林)及其相应的代谢产物青霉噻唑酸(氯唑青霉噻唑酸、乙氧萘青霉噻唑酸、苯唑青霉噻唑酸、青霉素V噻唑酸、羟氨苄青霉噻唑酸、青霉素G噻唑酸、氨苄青霉噻唑酸)残留的方法,并对市售乳制品中青霉素及青霉噻唑酸残留情况进行调查。方法乳制品样品中青霉素及青霉噻唑酸采用纯水超声提取,经乙腈沉淀蛋白,正己烷液液萃取除去脂肪,用氮气吹至近干,用乙腈+水(10+90)复溶后,经0.22μm微孔滤膜过滤,经高效液相色谱C18柱分离,选用乙腈(含0.1%甲酸)-水(含0.1%甲酸)为流动相,18 min内梯度洗脱分离7种青霉素及相应青霉噻唑酸共14种组分;在优化的质谱条件下,采用ESI源、正离子模式、多反应监测方式,外标法定量。结果方法的线性范围为1.0~200μg/kg,7种青霉素及相应青霉噻唑酸在各种乳制品基质中均有良好的线性关系(r>0.9991),方法最低检测限为0.03~0.15μg/kg;方法回收率在80.0%~110.0%,相对标准差为0.42%~7.06%。结论该方法测定7种青霉素药物及相应代谢产物青霉噻唑酸的残留量简便、快速、准确,可以满足对青霉素残留的监测要求。
OBJECTIVE To establish a HPLC-MS / MS method for the determination of seven penicillin antibiotics (cloxacillin, nafcillin, oxacillin, penicillin V, amoxicillin, penicillin G and ampicillin) in dairy products and The corresponding metabolites penicillifiazate (penzolethiazole thiazole acid, penicillin ethylpenicillin, oxacillin thiazole acid, penicillin V thiazole acid, amoxicillin thiazole acid, penicillin G thiazole acid, ampicillin Penicillin thiazole acid) residue method, and commercial dairy products penicillin and penicillin residues were investigated. Methods The penicillin and penicillin in dairy products were extracted with pure water by ultrasonic wave. The protein was precipitated by acetonitrile and extracted by liquid-liquid extraction with n-hexane. After the solution was flushed with nitrogen to near dryness and reconstituted with acetonitrile + water (10 + 90) 0.22μm microporous membrane filtration, the high performance liquid chromatography C18 column separation, the choice of acetonitrile (containing 0.1% formic acid) - water (containing 0.1% formic acid) as the mobile phase within 18 min gradient elution of seven kinds of penicillin and corresponding blue Fungi thiazole acid a total of 14 components; under the optimized mass spectrometry conditions, the use of ESI source, positive ion mode, multiple reaction monitoring, external standard method. Results The linear range of the method was 1.0 ~ 200μg / kg. There was a good linear relationship between the seven kinds of penicillins and the corresponding penicillin in various dairy products (r> 0.9991). The detection limit was 0.03 ~ 0.15μg / kg; the recovery rate was between 80.0% and 110.0%, and the relative standard deviation was between 0.42% and 7.06%. Conclusion The method for the determination of penicillin 7 penicillin drugs and the corresponding metabolites of penicillin thiazole acid residue is simple, fast and accurate, to meet the monitoring requirements of penicillin residues.