海产品、底泥、海水中扑草净药物残留量的液相色谱-串联质谱检测

Determination of Prometryne Residues in Seafood,Sediment,Seawater by Liquid Chromatography Tandem Mass Spectrometry

建立了海产品、底泥、海水中扑草净药物残留量的液相色谱-串联质谱检测方法。对海产品、底泥样品,采用快速溶剂提取仪(ASE)乙腈提取,凝胶渗透色谱(GPC)净化,液质联用仪(LC-MS/MS)分析;对海水样品采用酸化乙腈提取,氨基固相萃取柱净化,LC-MS/MS分析。实验结果显示,扑草净在浓度0.025～8.0ng/mL时,线性关系良好(R2=0.9999);海产品、底泥样品的方法测定低限为0.25μg/kg,3个加标水平下的平均回收率为90.0%～105.4%,相对标准偏差(RSD)为2.9%～5.3%;海水样品的方法测定低限为0.50μg/L,3个加标水平下的平均回收率为79.5%～99.6%,RSD为3.4%～11.9%。该方法简单、快速、准确,可用于海产品、底泥、海水样品中扑草净的筛选和测定。

The liquid chromatography tandem mass spectrometry （LC-MS/MS） methods have been established for the determination of prometryne residues in seafood, sediment and seawater, respectively. The seafood and sediment samples were extracted with aeetonitrile by ASE, coupled with gel permeation chromatography （GPC） clean-up, and then detected by LC-MS/MS. The sea water samples were extracted with acidified acetonitrile, purified by NH2 SPE column, and then detected by LC-MS/MS. Results showed that good linear was obtained in the concentration range of 0. 025 - 8.0ng/mL with a correlation coefficient of 0. 9999. The method was carried out at three spiking levels, the average recoveries were 90. 0% - 105.4% for seafood and sediment samples with RSD of 3.9% - 18.0% ,and 79. 5% -99. 6% for seawater samples with the RSD of 3.4% - 11.9%. The LOD of prometryne was 0. 5 txg/L in seawater and O. 25tzg/kg in seafood and sediment. The method is sample, fast and credible, so it can be applied to screening and determination of prometryne in seafood, sediment and seawater samples.