超高效液相色谱-串联质谱法测定牛奶中4种β-内酰胺类抗生素及其主要代谢产物

Determination of 4 kinds of β-lactam antibiotics and their main metabolites in milk by ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  β-内酰胺类抗生素  牛奶  超高效液相色谱-串联质谱法

英文关键词:β-lactam antibiotics  milk  ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测牛奶中青霉素G、青霉素V、氨苄西林、阿莫西林及其代谢产物脱羧噻唑酸含量的分析方法。方法 样品经0.2%氨水乙腈溶液超声离心提取, 通过Oasis PRiME HLB固相萃取柱进行净化, 采用超高效液相色谱-串联质谱法进行测定。结果 青霉素G、青霉素V、氨苄西林、阿莫西林及其代谢产物脱羧噻唑酸在所考察的线性范围内线性良好, 相关系数不低于0.999; 方法回收率为70.9%~101.6%, 相对标准偏差(relative standard deviation, RSD)为4.0%~7.5%。市售的35份样品中, 均未检出青霉素G、青霉素V、阿莫西林、氨苄西林及其代谢产物。结论 该方法操作简单、重现性好, 可用于牛奶中青霉素G、青霉素V、阿莫西林、氨苄西林及其代谢产物脱羧噻唑酸的检测。

英文摘要:

      Objective To establish a analytical method for the determination of penicillin G, penicillin V, ampicillin, amoxicillin and their metabolites decarboxythiazolinic acid in milk by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the target compound were extracted from sample by 0.2% ammonia acetonitrile solution and purified by solid-phase extraction with Oasis PRiME HLB, and the samples were analyzed by UPLC-MS/MS. Results The linearity of penicillin G, penicillin V, ampicillin, amoxicillin and their metabolites decarboxythiazolinic acid was good within the investigated linear range, and the correlation coefficients were not less than 0.999; the recoveries of the method were 70.9%?101.6% and the relative standard deviations were 4.0%?7.5%. Penicillin G, penicillin V, amoxicillin, ampicillin, and their metabolites were not detected in 35 commercially available samples. Conclusion This method is simple and reproducible, and can be used for the detection of penicillin G, penicillin V, amoxicillin, ampicillin and their metabolites decarboxythiazolic acid in milk.