液相色谱串联质谱法测定水产品中的敌百虫残留量

将水产品样品经乙腈提取,正已烷除脂,旋转浓缩后采用液相色谱串联质谱法进行定性、定量分析。线性范围为5—100μg/kg,线性相关系数为0.9987,定性检出限1.7μg/kg,定量检出限3.5μg/kg。在鳗鱼、虾和罗非鱼3种不同样品基质中进行添加浓度为10,20,50μg/kg的验证实验,回收率在77.2%—87.5%之间,相对标准偏差(RSD)在5.4%—8.3%之间,并对敌百虫的质谱裂解进行了分析。本法快速简单,高效,灵敏度高,符合检测要求。

Determination of Trichlorfon Residue in Aquatic Products by Liquid Chromatography- Mass Spectrometry

The compound was extracted with acetonitrile and cleaned with hexane,and concentrated with rotary evaporation.The treated sample solution was qualitatively and quantitatively analyzed by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The linear range was between 5 and 100μg/kg with coefficient correlation of 0.9987,and the detection limit was 1.7μg/kg with the quantification limit of 3.5μg/kg.The demonstration test was carried out in different samples(such as eel,shrimp and tilapia fish) at additional concentration of 10,20,50μg/kg,and the recoveries were in the range of 77.2%—87.5%,and RSD were from 5.4% to 8.3%,then the MS fragmentation mechanism of this compound was analyzed.The method is effective,fast and high sensitivity,and that meets the request of detection.