分子印迹固相萃取-超高效液相色谱-串联质谱法测定牛奶中11种氨基糖苷类抗生素

Determination of 11 kinds of aminoglycosides in milk by molecularly imprinted solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  氨基糖苷类抗生素  分子印迹固相萃取  超高效液相色谱-串联质谱法  牛奶

英文关键词:aminoglycosides  molecularly imprinted solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  milk

中文摘要:

      目的 建立分子印迹固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测牛奶中11种氨基糖苷类抗生素(巴龙霉素、妥布霉素、庆大霉素、卡那霉素、阿米卡星、安普霉素、链霉素、双氢链霉素、新霉素、壮观霉素、潮霉素B)残留的测定方法。方法 样品经5%三氯乙酸-乙腈提取, 氨基糖苷类分子印迹聚合物(molecular imprinted polymers, MIPs)固相萃取柱净化, SiELC Obelisc R色谱柱分离, 采用超高效液相色谱-串联质谱仪进行测定。结果 方法检出限为1.0~ 5.0 μg/kg, 定量限为2.0~10.0 μg/kg。11种氨基糖苷类药物在1.0~500.0 μg/kg范围内关系良好(r2≥0.9911), 牛奶中加标回收率为70.7%~115.6%, 相对标准偏差(relative standard deviations, RSDs) (n=6)为1.1%~9.8%。结论 本方法准确度、灵敏度高, 可用于牛奶中11种氨基糖苷类抗生素的同时检测。

英文摘要:

      Objective To establish a method for the determination of 11 kinds of aminoglycosides (paromomycin, tobramycin, gentamicin, kanamycin, amikacin, apramycin, streptomycin, dihydrostreptomycin, neomycin, spectinomycin, hygromycin B) in milk by molecularly imprinted solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 5% trichloroacetic acid-acetonitrile, cleaned up by a molecular imprinted polymers (MIPs) solid phase extraction column, and separated by a SiELC Obelisc R column using an ultra performance liquid chromatography-tandem mass spectrometer. Results The limits of detection were 1.0?5.0 μg/kg, and the limits of quantitation were 2.0? 10.0 μg/kg. The relationships of the 11 kinds of aminoglycosides were good within the range of 1.0-500.0 μg/kg (r2≥0.9911), the recoveries of spiked milk were 70.7%?115.6%, and the relative standard deviations (RSDs) (n=6) were 1.1%–9.8%. Conclusion This method is accurate and sensitive, and can be used for the simultaneous determination of 11 kinds aminoglycosides in milk.