红茶中56种农药残留的GC-MSMS定时SRM测定方法.pdfVIP

现代食品科技 Modern Food Science and Technology 2013, Vol.29, No.5 红茶中56 种农药残留的GC-MS/MS 定时SRM 测定方法 陈立伟，王斌，刘春生，罗东辉，陈意光，韩婉清 （广州市质量监督检测研究院，国家加工食品质量监督检验中心（广州），广州市食品安全检测技术重点实验室， 广州市食品安全风险动态监测与预警研究中心，广东广州 510110） 摘要：建立了红茶中甲胺磷等 56 种农药残留的气相色谱-三重四级杆串联质谱 （GC-MS/MS）测定方法。实验考察了不同提取 剂的提取效果，比较了Cleanert TPT 固相萃取柱和QuEChERS 的净化效果，优选出以正己烷:丙酮= （7:3，V/V ）提取，Cleanert TPT 固相萃取柱净化的实验条件；采用优化的GC-MS/MS “定时SRM ”模式进行测定，有效解决色谱保留时间出现偏移的问题。结果表 明：与QuEChERS 净化相比，经TPT 柱净化后，54 种农药信噪比提高了2 倍以上；56 种农药的检出限为 1~18 μg/kg。在3 μg/kg~600 μg/kg 范围内，进行3 个浓度水平的加标回收实验，除甲胺磷外，其余 55 种农药的平均回收率为 73~126%，相对标准偏差（RSD ， n=6 ）小于18%。本方法提取、净化效果良好，检测准确、灵敏、高效，适合红茶中56 种农药残留的测定。 关键词：红茶；农药残留；固相萃取；气相色谱-三重四级杆串联质谱；定时SRM 文章篇号：1673-9078(2013)5-1136-1143 Determination of 56 Pesticides in Black Tea by GC-MS/MS with Timed SRM CHEN Li-wei, WANG Bin, LIU Chun-sheng, LUO Dong-hui, CHEN Yi-guang, HAN Wan-qing (Guangzhou Quality Supervision and Testing Institute, National Centre for Quality Supervision and Testing of Processed Food (Guangzhou), Guangzhou Key Laboratory of Testing Technology for Food Safety, Guangzhou Research Center for Food Safety Risk Monitoring and Rapid Alert, Guangzhou, Guangdong, 510110, China) Abstract: A novel method was developed for simultaneous determination of methamidophos and other 55 pesticides in black tea using gas chromatography -triple quadrupole mass spectrometry (GC-MS/MS). The extraction effects of different extraction regents were compared and the purifying effect s of Cleanert TPT Solid phase extraction column and QuEChERS were also investigated. The optimum pretreatment conditions for the tea samples were determined as follows: extractingthe tea samp les by n-hexane: acetone (7:3, V/V) followed by Cleanert TPT column purification. After purifi