Saito-Shida Shizuka, Nemoto Satoru, Teshima Reiko
a Division of Foods, National Institute of Health Sciences , Tokyo , Japan.
J Environ Sci Health B. 2015;50(11):760-76. doi: 10.1080/03601234.2015.1058092.
An efficient and reliable GC-MS/MS method for the multiresidue determination of pesticides in tea was developed by modifying the Japanese official multiresidue method. Sample preparation was carefully optimized for the efficient removal of coextracted matrix components. The optimal sample preparation procedure involved swelling of the sample in water; extraction with acetonitrile; removal of water by salting-out; and sequential cleanup by ODS, graphitized carbon black/primary secondary amine (GCB/PSA) and silica gel cartridges prior to GC-MS/MS analysis. The recoveries of 162 pesticides from fortified (at 0.01 mg kg(-1)) green tea, oolong tea, black tea and matcha (powdered green tea) were mostly (95-98% of the tested pesticides) within the range of 70-120%, with relative standard deviations of <20%. Poor recovery of triazole pesticides was considered to be due to low recovery from the silica gel cartridges. The test solutions obtained by the modified method contained relatively small amounts of pigments, caffeine and other matrix components and were cleaner than those obtained by the original Japanese official multiresidue method. No interfering peaks were observed in the blank chromatograms, indicating the high selectivity of the modified method. The overall results suggest that the developed method is suitable for the quantitative analysis of GC-amenable pesticide residues in tea.
通过改进日本官方多残留方法,建立了一种高效可靠的气相色谱 - 串联质谱法(GC-MS/MS)用于茶叶中多种农药残留的测定。对样品制备进行了仔细优化,以有效去除共萃取的基质成分。最佳样品制备程序包括将样品在水中溶胀;用乙腈萃取;通过盐析去除水分;以及在进行GC-MS/MS分析之前,依次通过ODS、石墨化炭黑/ primary secondary amine(GCB/PSA)和硅胶柱进行净化。从添加了0.01 mg kg⁻¹农药的绿茶、乌龙茶、红茶和抹茶(粉状绿茶)中回收162种农药,大部分(占测试农药的95 - 98%)回收率在70 - 120%范围内,相对标准偏差<20%。三唑类农药回收率较低被认为是由于从硅胶柱中的回收率低。通过改进方法获得的测试溶液含有相对少量的色素、咖啡因和其他基质成分,比通过原始日本官方多残留方法获得的溶液更纯净。在空白色谱图中未观察到干扰峰,表明改进方法具有高选择性。总体结果表明,所建立的方法适用于茶叶中可进行气相色谱分析的农药残留的定量分析。