液相色谱质谱联用法测定水产品中泰乐菌素残留方法的研究

为了建立鱼、虾中泰乐菌素残留量的液相色谱串联质谱检测方法，文章通过对液相色谱和质谱条件、预处理、分离、纯化方法的探讨，确定了以罗红霉素为内标，先用乙腈提取，中性氧化铝柱净化，加异丙醇旋转蒸发至于，定容，过膜，上机测试。所建立的分析方法，泰乐菌素在1．0～500ng·mL。质量浓度范围内呈良好的线性关系，相关系数均大于0．998，检出限为0．5μg·kg-1，定量限为1．0μg·kg-1。经过验证，在鲫（CarassiusauFatus）、对虾（Penacusorientalis）和草鱼（Ctenopharyngodonidellus）3种样品中的加标试验，3个不同质量浓度水平的加标回收率为82．40％-100．70％，相对标准偏差为0．86％～5．82％，符合对水产品中药物残留检测的技术要求。

Study on LC-MS/MS method for determination of Tylosin residues in aquatic products

To establish LC-MS/MS method for the determination of Tylosin residues in aquatic products, we optimized the LC and MS conditions, pretreatment, separation and purification, used roxithromycin as internal standard and acetonitrile as extraction solution, purified the neutral alumina column, rotarily evaporated with isopropyl alcohol, dissolved and filtered, and finally injected into the in- strnment. The established method has a good linear relationship in the concentration range from 1.0 ng＇mL-1 to 500 ng＇mL-~ with coef- ficient greater than 0. 998. The LOD and LOQ are O. 5 t~g.kg-1 and 1.0 ~g.kg-1 , respectively. Moreover, we designed 3 spike tests with different concentrations in Carassius auratus, Penacus orientalis and Ctenopharyngodon idellus, and it is proved that their recover- ies of standard addition and RSDs are 82.40% - 100. 70% and 0. 86% ~ 5.82%, respectively.