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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。
A liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of prometryne in seafood, sediment and seawater was established. The samples of marine products and sediments were analyzed by acetonitrile extraction, gel permeation chromatography (GPC) and liquid chromatography mass spectrometry (LC-MS / MS). The samples of seawater were extracted with acidified acetonitrile, Amino solid phase extraction column, LC-MS / MS analysis. The experimental results showed that prometryn had a good linear relationship (R2 = 0.9999) at the concentration of 0.025-8.0ng / mL, the lower limit of determination of seafood and sediment samples was 0.25μg / kg, and the three spiked levels The average recoveries ranged from 90.0% to 105.4%, and the relative standard deviations (RSDs) ranged from 2.9% to 5.3%. The lower limit of determination for seawater samples was 0.50μg / L, and the average recovery was 79.5% 99.6%, RSD 3.4% ~ 11.9%. The method is simple, rapid and accurate and can be used for the screening and determination of prometryne in seafood, sediment and seawater samples.