超高效液相色谱-串联质谱法快速测定浓缩果汁中噻菌灵和多菌灵的残留量

Rapid determination of thiabendazole and carbendazim in concentrated fruit juices by ultra-high performance liquid chromatography-tandem mass spectrometry

建立了同时测定浓缩果汁中噻菌灵和多菌灵残留的超高效液相色谱-串联质谱快速检测法。样品用乙酸乙酯提取,以ACQUITY UPLC BEH C18色谱柱（50 mm×2.1 mm,1.7μm）进行超高效液相色谱分离,以电喷雾电离串联质谱正离子多反应监测（MRM）模式进行测定,以基质匹配标准溶液外标法定量。结果表明：在试验条件下,噻菌灵和多菌灵在0.5-10μg/kg范围内线性关系良好,相关系数大于0.99,不同基质中的检出限（S/N=3）范围为0.12-0.23μg/kg。在0.5、1.0和5.0μg/kg 3个水平下噻菌灵和多菌灵的加标回收率为76.98%-108.7%,相对标准偏差（RSD）为2.95%-9.99%。同时,本研究对浓缩果汁中噻菌灵和多菌灵残留检测的基质效应进行了考察。本方法具有操作简便、快速、准确的特点,可用于浓缩果汁中噻菌灵和多菌灵残留量的日常检测。

A method was developed for the rapid determination of thiabendazole and carbenda-zim residues in concentrated fruit juices by using ultra-high performance liquid chromatography （ UHPLC）coupled with triple quadrupole tandem mass spectrometry（ MS/MS）,and quantified by matrix-matched standard solution in external standard method. The residues in the samples were extracted by ethyl acetate,and then analyzed by using UHPLC-MS/MS in multiple reac-tion monitoring（ MRM）mode via positive electrospray ionization with an Waters ACQUITY UP-LC BEH C18 column（50 mm×2. 1 mm,1. 7 μm）as the analytical column. Good linearities were obtained in the range of 0. 5-10 μg/kg for both pesticides with correlation coefficients greater than 0. 99. The recovery experiments were carried out by spiking standards into blank samples of apple,peach,orange,pear,grape juices at three levels of 0. 5,1. 0 and 5. 0 μg/kg. The recoveries of thiabendazole and carbendazim were from 76. 98% to 108. 7% with the relative standard deviations（ RSD）of 2. 95%-9. 99%. For both pesticides in different matrices,the lim-its of detection（ S/N=3）were in the range of 0. 12-0. 23 μg/kg. Meanwhile,the pyrolysis mechanism and matrix effects for the determination of thiabendazole and carbendazim in con-centrated fruit juices were investigated in this study. The method is simple,rapid and accurate, and can be used for the routine analysis of thiabendazole and carbendazim in concentrated fruit juices.