超高效液相色谱-串联质谱法快速确证水产品中喹乙醇残留量

A rapid confirming method of olaquindox residue in aquatic products by UPLC- MS /MS

根据喹乙醇见光快速分解的特性,建立了快速确证水产品中喹乙醇残留量的方法。为减少样品中喹乙醇的分解,实验操作均在避光条件下进行。样品经乙腈-乙酸乙酯（1∶1,V/V）提取,无水硫酸钠去除水分,取1/5提取液进行氮吹,尽量缩短浓缩时间,正己烷去除脂肪后,采用超高效液相色谱-串联质谱测定喹乙醇。乙腈-5 mmol/L乙酸铵（含0.05%甲酸）溶液为流动相,采用ESI＋,多反应监测（MRM）,外标法定量,快速确证样品中喹乙醇残留。方法检出限为1μg/kg,在1～100μg/L浓度范围内线性关系良好,相关系数为0.999 4,方法的回收率在71.5%～89.6%之间,相对标准偏差小于15%。本方法快速、准确、简便,灵敏度可满足中国限量要求,为水产品日常监测工作提供经济、快速的参考技术。[中国渔业质量与标准,2014,4（3）：29-33]

A rapid method was developed for confirming olaquindox residue in aquatic products based on its character- istics of being decomposed quickly in light. In order to avoid the decomposition of olaquindoxin, all samples were test- ed away from light before determined by UPLC - MS/MS, samples were extracted with acetonitrile - ethylacetate （1： 1, V/V） ; water in the sample was removed by anhydrous Na2 SO4; one fifth of the solvent was vaporized by nitro- gen blowing as shortening the concentration time, and finally fat in the sample were defatted by hexane. Choosing ace- tonitrile - 5 mmol/L ammonium acetate solution （ containing 0.05 % of formic acid） as mobile phase, Electrospray ion （ESI）, Multiple reaction monitoring （MRM） as equipment parameters, external standard method as quantifica- tion. The detection limit of the method was 1 μg/kg. The liner relationship was fine in the range of 1 to 100 μg/L with correlation coefficient of 0.999 4 the recovery rate ranging between 71.5% and 89.6%, and relative standard devia- tion less than 15%. The accuracy, precision, convinence economical and fast technical method for daily control and Quality and Standards, 2014, 4（3）：29-333 and sensitivity of the method are satisfactory, thus it is an monitoring the safety of aquatic products. [ Chinese FisheryQuality and Standards, 2014, 4（3）：29-33J