超高效液相色谱串联质谱法测定茶叶、茶汤和土壤中氟环唑、茚虫威和苯醚甲环唑残留  

Residue Determination of Epoxiconazole,Indoxacarb and Difenoconazole in Tea,Tea Infusion and Soil using Ultra High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry

作　　者：张新忠[1,2,3] 罗逢健[1,2,3] 陈宗懋[1,2,3] 刘光明[1,2,3] 楼正云[1,2,3] 王方[1] 吴鲁超[1] 

机构地区：[1]中国农业科学院茶叶研究所农产品质量安全研究中心,杭州310008 [2]农业部茶及饮料植物产品加工与质量控制重点开放实验室,杭州310008 [3]农业部茶叶产品质量安全风险评估实验室,杭州310008

出　　处：《分析化学》2013年第2期215-222,共8页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学青年基金项目(No.21107137);国家茶叶产业技术体系项目(No.CARS-23);浙江省自然科学基金项目(No.Y3100259)资助

摘　　要：建立了绿茶、红茶、普洱茶、茶鲜叶、红茶汤和土壤中氟环唑、茚虫威、苯醚甲环唑残留分析方法。采用Florisil与GCB混合柱净化茶叶和土壤,BondElut C18固相萃取柱富集净化茶汤,超高效液相色谱串联质谱法测定,并对3种农药的质谱裂解和基质效应进行了研究探讨。在0.005～4.0 mg/L浓度范围内均满足线性关系,r>0.9997,仪器检出限LOD<0.002 mg/L;在高、中、低3个添加浓度水平下,不同基质样品(绿茶、红茶、普洱茶、红茶汤、茶鲜叶和土壤)中平均回收率为66.3%～111.5%;相对标准偏差为0.85%～17.6%(n=6);方法定量限LOQ分别为0.005 mg/kg(成茶)、0.002 mg/kg(茶鲜叶、土壤)和0.10!g/L(茶汤)。采用此方法检测40份红茶、绿茶出口样品,1份检出茚虫威残留量为0.014 mg/kg;4份检出苯醚甲环唑残留量为0.012～0.040mg/kg,均未检出氟环唑残留。采用此方法进行茚虫威在茶鲜叶-绿茶加工过程中的消解率、茶叶-茶汤冲泡过程中的浸出率研究,表明茚虫威在绿茶加工过程中的平均消解率为24.8%,3次冲泡的总浸出率平均值为5.2%。To meet the need of simultaneous residue determination for epoxiconazole, indoxacarb and difenoconazole in tea, tea infusion and soil, a sensitive and convenient method was developed by validated using ultra-high performance liquid chromatography coupled with tandem mass spectrometry （UPLC-MS/MS）. Target compounds were extracted by acetonitrile followed by Florisil and graphit carbon black （GCB） mix-column cleanup for tea and soil, and target compounds in tea infusion was extracted and cleanuped by BondElut CIs-SPE column. The fragmentation pathway and matrix effect were investigated. Over the concentration in the range of 0. 005-4. 0 mg/L for epoxiconazole, indoxacarb and difenoconazole, the correlation coefficients （r） of the calibration curves were above 0.9997, and the limits of detection （LODs） were lower than 0. 002 mg/L. The average recoveries of epoxiconazole, indoxacarb and difenoconazole in difierent matrix （ green tea, black tea, puerh tea, black tea infusion, fresh tea leave and soil） at three spiked concentration levels ranged from 66.3 % to 111.5 % with relative standard deviations （RSDs） between 0.9% and 17.6% （n=5）. The limits of quantitation （LOQs） of three pesticides were lower than 0. 005 mg/kg in made tea, 0. 002 mg/kg in fresh tea leave and soil, 0.10 ug/L in black tea infusion. The proposed method was successfully applied to the routine export green tea and black tea sample （n = 40） in China, there were 0.014 mg/kg residue of indoxacarb in one sample, 0. 012 mg/kg-0. 040 mg/kg residue of difenoconazole in four sample, and no epoxiconazole detected, all of tea sample were meet the MRL requirements of EU and Japan. Also, this method was successfully used to the study on the degradation loss rate of indoxacarb during the processing of fresh tea leaves to made tea, and on the leaching rate of indoxacarb during the brewing process from made tea to tea infusion, the average results were the processing degradation loss rate of indoxacarb at 24.8% , and the total

关 键 词：农药残留 超高效液相色谱串联质谱法 茶叶 土壤 氟环唑 茚虫威 苯醚甲环唑 

分 类 号：TS272.7[农业科学—茶叶生产加工] O657.63[轻工技术与工程—农产品加工及贮藏工程]