QuEChERS-超高效液相色谱-串联质谱法同时测定水产品中20种苯并咪唑类药物及其代谢物残留

Simultaneous determination of 20 kinds of benzimidazoles and their metabolites residues in aquatic products by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

目的建立QuEChERS结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时快速测定水产品中20种苯并咪唑类药物及其代谢物残留量的分析方法。方法样品经乙腈提取,用乙二胺-N-丙基甲硅烷(primary secondary amine,PSA)和中性氧化铝吸附剂净化,通过Waters ACQUITY UPLC HSS T3 (2.1 mm×100 mm,1.8μm)色谱柱分离,以0.1%甲酸水溶液-乙腈为流动相,采用电喷雾正离子模式,多反应监测(multiple reaction monitoring,MRM)模式下分析,基质匹配曲线外标法定量。结果20种苯并咪唑类药物及其代谢物在0.05~20.00μg/L范围内线性关系良好(r^(2)≥0.9991),在空白样品基质中进行3个不同浓度水平的加标实验,平均回收率为63.3%~105.8%,相对标准偏差为0.1%~7.5%(n=6)。方法检出限为0.1~0.5μg/kg,定量限为0.3~2.0μg/kg。结论该方法操作简便、灵敏度高、准确可靠,适用于水产品中20种苯并咪唑类药物及其代谢物的快速筛查。

Objective To establish an analytical method for the simultaneous and rapid determination of 20 kinds of benzimidazoles and their metabolites residues in aquatic products by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The samples were extracted with acetonitrile, purified with primary secondary amine(PSA) and neutral alumina adsorbent, separated on a Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm, 1.8 μm) chromatographic column using 0.1% formic acid aqueous solution-acetonitrile as the mobile phase under the electrospray ionization mode, analyzed in multiple reaction monitoring(MRM) mode, and quantified by external standard method of matrix matching curve. Results The linear relationships of the 20 kinds of benzimidazoles and their metabolites were good within the range of 0.05-20.00 μg/L(r^(2)≥0.9991). The spiked experiments at 3 kinds of different concentration levels in the blank sample matrix were performed, and the average recoveries were 63.3%-105.8%, and the relative standard deviations were 0.1%-7.5%(n=6). The limits of detection were 0.1-0.5 μg/kg, and the limits of quantitation were 0.3-2.0 μg/kg. Conclusion This method has the advantages of simplicity, high sensitivity and good reliability, which is suitable for the rapid detection of 20 kinds of benzimidazoles and their metabolites residues in aquatic products.