QuEChERS-气相色谱质谱法快速测定水产品中扑草净残留

Rapid determination of prometryn in aquatic products by QuEChERS combined with gas chromatography mass spectrometry

    摘要
  • 摘要: 以QuEChERS作为样品前处理手段，建立测定水产品中扑草净残留的气相色谱-质谱法 (GC-MS)。样品以乙腈-二氯甲烷 (V∶V=8∶2) 混合溶液提取，提取液经吸附剂中性氧化铝、N-丙基乙二胺 (PSA)、纳米二氧化锆结合石墨化炭黑 (GCB) 净化后上机检测，内标法定量。结果显示，扑草净质量浓度介于5~200 μg·L−1线性关系良好，相关系数 (R2) 为0.9999。对草鱼 (Ctenopharyngodon idellus)、鳜 (Siniperca chuatsi)、中国对虾 (Penaeus chinensis)、海参 (Holothuria sp.) 和文蛤 (Meretrix meretrix) 进行4个水平的加标回收实验 (10、20、40和200 µg·kg−1)，方法的加标回收率为85.8%~111.8%，相对标准偏差为1.2%~8.8%，满足GB/T 27404—2008《实验室质量控制规范 食品理化检测》中实验室质量控制规范。扑草净的检出限 (LOD, S/N≥3) 和定量限 (LOQ, S/N≥10) 分别为5和10 µg·kg−1。该方法简单、快速、灵敏、净化效果好，能满足水产品中扑草净残留的检测需求。

     

    Abstract: A method was developed for the determination of prometryn in aquatic products by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with gas chromatography mass spectrometry. The samples were extracted by acetonitrile-dichloromethane mixture (V:V=8:2) and purified by neutral alumina, zirconium dioxide, PSA and GCB, quantified with internal standard. Good linearity was obtained in the range of 5.00−200 µg·L−1 with the correlation coeficient of 0.9999. The average recoveries were 85.8%−111.8% in Ctenopharyngodon idellus, Siniperca chuatsi, Penaeus chinensis, Holothuria sp. and Meretrix meretrix at four spiked levels of 10, 20, 40 and 200 µg·kg−1 with RSDS of 1.2%−8.8%, which meets the quality control specifications required in the national standard (GB/T 27404−2008 Criterion on Quality Control of Laboratories-Chemical Testing of Food). The limits of detection (S/N≥3) and quantification (S/N≥10) were 5.0 and 10.0 µg·kg−1, respectively. The method is suitable for the rapid determination of the prometryn residues in aquatic products owing to its advantages of simplicity, sensitivity, accuracy and better purification.

     

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