液相色谱串联质谱法检测草鱼中地西泮优化实验研究

Determination of diazepam residues in grass carp using liquid chromatography tandem mass spectrometry

本文旨在建立一种前处理操作简便、回收率较高的检测水产品中地西泮残留量的液相色谱-串联质谱法(LC-MS/MS)。以草鱼样品为例,样品经过3%氨水乙酸乙酯提取,平行旋转蒸发浓缩、中性氧化铝固相萃取柱(Alumina-N SPE)净化,采用外标法进行定量分析。结果表明:本方法操作简便,在草鱼样品中的方法回收率为82.0%~93.6%,相对标准偏差小于5%;当草鱼样品中地西泮的含量为2.34μg·kg^(-1)时,其扩展不确定度为0.16μg·kg^(-1)(k=2)。在实际检测应用中,回收率能够稳定在80%以上,批内相对标准偏差≤5%,批间相对标准偏差≤10%,因此该方法适用于鲤鱼、鲫鱼、鲢鱼、鳙鱼、草鱼等水产品中地西泮的检测。

In order to establish a Liquid Chromatography-Tandem Mass Spectrometry(LC-MS/MS)method for the detection of diazepam residues in aquatic products with simple pretreatment operation and high recovery rate,taking grass carp products samples as a case study,the samples were extracted by 3%ammonia-ethyl acetate,followed by parallel rotary evaporation for concentration,purified using neutral alumina solid phase extraction column(Alumina N SPE).Quantitative analysis was performed using external standard method.The results showed that the method was easy to operate,with the recovery rates of the method in grass carp samples ranging from 82.0%to 93.6%,and the relative standard deviation was less than 5%.When the diazepam content in grass carp samples was 2.34μg·kg^(-1),its expanded uncertainty was 0.16μg·kg^(-1)(k=2).In practical application,the recovery rate remained stable at over 80%,with an intra-batch relative standard deviation was less than 5%,and the inter-batch relative standard deviation was less than 10%,so the method was suitable for the detection of diazepam in various aquatic products,including carp,crucian carp,silver carp,bighead carp and grass carp.