超高效液相色谱-三重四级杆串联质谱法检测牛奶及其制品中恩诺沙星、头孢拉定、阿莫西林和氯霉素残留

Determination of enrofloxacin,cefradine,amoxicillin and chloramphenicol residues in milk and its products by UPLC-MS/MS

目的:建立超高效液相色谱-三重四级杆串联质谱法检测牛奶及其制品中恩诺沙星、头孢拉定、阿莫西林和氯霉素残留的分析方法。方法:取牛奶或牛奶制品,置加速溶剂萃取池中,加硅藻土,混合均匀后,置全自动加速溶剂萃取仪中,萃取溶剂选择甲醇-乙腈=2∶1(V∶V)进行提取;萃取完毕后,萃取液置塑料离心管中,低温离心10 min,上清液转移至GPC净化瓶中进行净化;净化液准确移取10 mL,4水浴氮吹至近干,加1 mL甲醇溶解,涡旋,滤过,超高效液相色谱-三重四级杆串联质谱仪定性、定量检测。结果:恩诺沙星、头孢拉定、阿莫西林和氯霉素在0.01~6.0μg/mL范围内线性良好,方法检出限分别为0.011、0.008、0.007、0.010μg/L,加标回收率(三水平)在85.4%~103.6%范围内。结论:实验结果表明,此方法具有自动化程度高、检测结果准确度高等优点,适用于牛奶及其制品中常见抗生素残留的监测。

Take milk or milk products,put them into the accelerated solvent extraction tank,add diatomite,mix evenly,and put them into the automatic accelerated solvent extraction instrument. The extraction solvent is methanol acetonitrile=2∶1(V∶V). After extraction,the extract is placed in a plastic centrifuge tube,centrifuged at low temperature for 10 minutes,and the supernatant is transferred to a GPC purification bottle for purification. Accurately transfer 10 ml of purified solution,blow nitrogen in 4 water baths to nearly dry,add 1 ml of methanol to dissolve,vortex,filter,and conduct qualitative and quantitative detection by ultra-high performance liquid chromatography triple four-stage rod tandem mass spectrometry. The linearity of enrofloxacin,cefradine,amoxicillin and chloramphenicol are good in the range of 0. 01-6. 0 μg/mL,and the detection limits are 0. 011 μg/kg,0. 008 μg/kg,0. 007 μg/kg and 0. 010 μg/kg,the recovery rates(three levels)are in the range of 85. 4% — 103. 6%. This method has the advantages of high automation and high accuracy,and is suitable for the monitoring of common antibiotic residues in milk and its products.