高效液相色谱法测定水产品中喹乙醇代谢物残留量  

Determination of Olaquindox Metabolite Residues in Fishery Products by High Performance Liquid Chromatography

作　　者：贝亦江[1] 王扬[1] 何丰[1] 任胜兰[2] 

机构地区：[1]浙江省水产质量检测中心,浙江杭州310012 [2]浙江科技学院生物与化学工程学院,浙江杭州310023

出　　处：《食品科学》2013年第10期255-258,共4页Food Science

基　　金：浙江省科技厅水产品加工产业团队课题(2011R09031-10)

摘　　要：建立高效液相色谱法对水产品中喹乙醇代谢物(3-甲基喹噁啉-2-羧酸)残留量的检测方法。样品用2.0mol/L的盐酸水解,固相萃取净化,反相色谱柱分离,紫外检测器检测,外标法定量。喹乙醇代谢物在质量浓度0.01～1.0μg/mL的范围内呈线性关系,相关系数为0.9998,检出限为4.0μg/kg,定量限为12.0μg/kg。喹乙醇代谢物回收率在71.0%～86.5%之间,相对标准偏差在3.84%～7.32%之间。对样品前处理过程进行优化,增加提取步骤、缩短酸解时间后,回收率平均提高6.4%;同时发现,不过滤比过滤的回收率平均提高13.0%。A high performance liquid chromatography method was established to determine olaquindox metabolite （3-methyl-2-quinoxalinecarboxylic acid, MQCA） residues in fishery products in this study. Olaquindox metabolite residues were extracted with 2 mol/L hydrochloric acid, and purified on an SPE column. Sample analysis was performed using RP-HPLC and external standard method. In the concentration range of 0.01 to 1.0 ~tg/mL, an excellent linearity was observed with a correction coefficient of 0.9998. The LOD （limit of detection） was 4.0 ~tg/kg and LOQ （limit of quantification） was 12.0 ~tg/kg. Average recovery rates for different species of fishery products spiked at three levels varied between 71.0% and 86.5% with a RSD of 3.84% to 7.32%. The recovery of MQCA was increased by an average of 6.4% under optimized pretreatment conditions with more complicated extraction procedure and shortened oscillation time. Moreover, an average increase of 13.0% in MQCA recovery was obtained by omitting filtration.

关 键 词：高效液相色谱 水产品 喹乙醇代谢物 

分 类 号：S912[农业科学—水产科学]