冻干鲤鱼粉中恩诺沙星和环丙沙星残留测定的两种前处理-食品科学.PDFVIP

※分析检测 食品科学 2011, Vol. 32, No. 02 227 1 1 1 1,2,3, 赵 艳 ，王丽敏 ，刘耀敏 ，张凤枰 * (1.通威股份有限公司，四川 成都 610041 ；2. 中国科学院西北高原生物研究所，青海 西宁 810001 ； 3. 中国科学院研究生院，北京 100049) 采用固相萃取和液液萃取结合超高效液相色谱 - 串联质谱法(UPLC-MS/MS) ，对冻干鲤鱼粉中恩诺沙星和 环丙沙星残留量进行测定，比较两种前处理方法的测定结果。固相萃取法：样品经 EDTA-Mcllvaine 缓冲溶液提 取，HLB 固相萃取柱净化，氮气浓缩；液液萃取法：样品经酸性乙腈溶液提取，正己烷液液萃取净化，旋转 蒸发浓缩。两种方法的提取液浓缩定容后，以超高效液相色谱 - 串联质谱仪测定，外标法定量。固相萃取和液液 萃取法的回收率分别为 95%～112% 和75%～90%，RSD 分别为2.9%～7.4% 和 1.0%～4.6% ，检出限分别为 1.0μg/kg 和 0.1 ～0.2 μg/kg 。结果表明，两种方法简便快速、重现性好、选择性强，均适用于鱼肉和冻干鲤鱼粉中恩诺沙 星和环丙沙星残留的测定。 恩诺沙星；环丙沙星；残留；冻干鲤鱼粉；超高效液相色谱 - 串联质谱法(UPLC-MS/MS) Comparison of Two Pretreatment Methods for UPLC-MS/MS Determination of Enrofloxacin and Ciprofloxacin Residues in Freeze-dried Carp Meal 1 1 1 1,2,3, ZHAO Yan ，WANG Li-min ，LIU Yao-min ，ZHANG Feng-ping * (1. Tongwei Co. Ltd., Chengdu 610041, China；2. Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810001, China；3. Graduate University of Chinese Academy of Sciences, Beijing 100049, China) Abstract ：Sample pretreatment was achieved by two different methods, solid-phase extraction and liquid-liquid extraction, before the analysis of enrofloxacin and ciprofloxacin residues in freeze-dried carp meal on UPLC-MS/MS. The analytical results were compared to examine if the two pretreatment methods influence the accuracy of determination. The solid-phase extraction procedure was compose