ASE萃取／GPC—SPE净化／GC—MS测定茶叶中的有机磷残留.doc

ASE萃取／GPC—SPE净化／GC—MS测定茶叶中的有机磷残留 王耀。张汉霞，邹潍力，刘少彬，谢翠美 (东莞市海洋与渔业环境监测站，广东东莞523079) 摘要：建立加速溶剂萃取一凝胶渗透色谱，固相萃取净化一气质法测定茶叶中的有机磷残留的分析方法。样品用丙酮一二氯甲烷(1：1)作为溶剂，加速溶剂提取，提取液经过凝胶渗透色谱除去大分子杂质后，再经过Carb／NH2柱净化后 供GC—FPD和GC—MS分析。方法检出限为为0．001mg／kg一0．0075mg／kg，在加标水平为0.050mg／kg时，回收率为76．3％．94．6％，相对标准偏差为2．4％,8．1％,方法具有自动化程度高、萃取效率高、净化效果好、精密度好，分析快速等优点，适用于茶叶中有机磷残留的日常检测工作。 关键词：加速溶剂萃取；凝胶渗透色谱；固相萃取；有机磷农药；茶叶 Determination of Organophosphrous Pesticides Residue in Tea Using ASE Extraction-GPC／SPE Purification GC-MS Analysis WANG Yao，ZHANG Han—xia，ZOU Wei—li，LIU Shao—bin，XIE Cui—mei (Dongguan Marine and Fishery Environment Monitoring Station，Dongguan523079，Guangdong，China) Abstract：A method for determination organophosphrous pesticides residues in tea sample was described by accelerated solvent extraction-gel permeation chromatography／solid phase extraction purification gas chromatography-mass spectrometr．The target anslytes were extracted With the solution of acetone／dichloromethane(1：1)usingaccelerated solventextraction(ASE), solid extraction．The anddeterminationof were (GPC)andCarb／NH2 phase separation analytesperformeby with andexternal the GC—FPDandGC-MS selectedion standardmethod．Under using monitoring(SIM)mode in with conditions．thedetection were the of0．001 5 mg／kg-0．007ms／ks optimal limits(S／N=3)ofpesticidesrange therelativestandarddeviationsof2．4％-8．1％．Therecoveriesof fromteas withmixed pesticides samplespiked efficientin standardsat0．050 from methodWas mg／kgranged 76．3％-94．6％．Therapid，precise，sensitive，hi is extractionconvenientand routine resultsindicatedthatthismethod purification．Afterapplications，the suitableforthe of resduesinthetea． determinationorganophosphrouspesicide solvent words：accelerated Key extraction(ASE)；gelpermeationchromatography(GPC)；sophase extraction(SPE)；organophosphrouspesticid；tea 茶叶以其抗癌、抗氧化、消除人体自由基等独特 的保健功效，深受世人喜爱，已成为仅次于碳酸饮料 和饮用水的世界第三大饮料。另一方面，随着人民生 活水平的目益提高，人们对茶叶中农药残留等质量安 全问题给予了高度关注。目前茶叶中农药残留的检测 方法主要有：气相色谱法【lI、液相色谱法121、气质法和 液质法141等。食品中有机磷残留农药的各种检测技术 中，GC和GC—MS方法以其快速、灵敏