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建立了乳及乳制品中13种β-受体激动剂类药物多残留的同位素内标-高效液相色谱串联质谱分析方法。样品经三氯乙酸沉淀蛋白,提取液经SupelcleanLC-SCX固相萃取柱净化后,用HPLC-MS/MS进行测定。采用AgilentEclipse Plus C18色谱柱(2.1×150 mm,3.5μm),0.1%甲酸水-乙腈流动相进行梯度洗脱,用电喷雾离子源正离子多反应监测(MRM)模式进行MS/MS检测。其中克伦特罗在0.05～5.0μg/kg线性范围内,其余12种分析物在0.25～10μg/kg线性范围内具有较好的线性关系,相关系数r>0.9988。方法检出限(LOD)为0.02～0.17μg/kg,定量限(LOQ)为0.05～0.48μg/kg。空白样品添加回收率为83.2%～102.6%,相对标准偏差为5.0%～13%。
A multi-residue isotope internal standard-high performance liquid chromatography-tandem mass spectrometry method was established for the determination of 13 β-agonists in milk and dairy products. The sample was precipitated by trichloroacetic acid, the extract was purified by SupelcleanLC-SCX SPE cartridge and determined by HPLC-MS / MS. The elution was performed on a Agilent Eclipse Plus C18 column (2.1 × 150 mm, 3.5 μm) using a mobile phase of 0.1% formic acid in acetonitrile. MS / MS was carried out using electrospray ionization positive ion MRM. Clenbuterol was in the linear range of 0.05 ~ 5.0μg / kg, and the other 12 analytes had a good linearity in the linear range of 0.25 ~ 10μg / kg with the correlation coefficient r> 0.9988. The method detection limit (LOD) was 0.02 ~ 0.17μg / kg, and the limit of quantification (LOQ) was 0.05 ~ 0.48μg / kg. The recoveries of blank samples were 83.2% ~ 102.6% with relative standard deviations of 5.0% ~ 13%.