Zheng Xiangping, Ding Liping, Chen Zhitao, Guo Jing, Zhang Rui, Wu Wenfan
Se Pu. 2015 Jun;33(6):652-6. doi: 10.3724/sp.j.1123.2015.01034.
A method was developed for the rapid determination of thiabendazole and carbendazim 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 reaction monitoring (MRM) mode via positive electrospray ionization with an Waters ACQUITY UPLC BEH C18 column (50 mm x 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 limits 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 concentrated 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.
建立了一种采用超高效液相色谱(UHPLC)与三重四极杆串联质谱(MS/MS)联用,以外标法用基质匹配标准溶液定量,快速测定浓缩果汁中噻菌灵和多菌灵残留量的方法。样品中的残留量用乙酸乙酯提取,然后采用UHPLC-MS/MS在多反应监测(MRM)模式下,通过正电喷雾电离,以Waters ACQUITY UPLC BEH C18柱(50 mm×2.1 mm,1.7 µm)为分析柱进行分析。两种农药在0.5 - 10 µg/kg范围内均获得良好的线性关系,相关系数大于0.99。通过向苹果汁、桃汁、橙汁、梨汁、葡萄汁的空白样品中分别添加0.5、1.0和5.0 µg/kg三个水平的标准品进行回收率实验。噻菌灵和多菌灵的回收率为76.98%至108.7%,相对标准偏差(RSD)为2.95% - 9.99%。对于不同基质中的两种农药,检测限(S/N = 3)在0.12 - 0.23 µg/kg范围内。同时,本研究还考察了浓缩果汁中噻菌灵和多菌灵测定的热解机理和基质效应。该方法简便、快速、准确,可用于浓缩果汁中噻菌灵和多菌灵的常规分析。