分散固相萃取-液相色谱质谱/质谱检测茶叶中吡虫啉、啶虫脒、茚虫威和氯虫苯甲酰胺农药残留
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摘要
目的建立应用分散固相萃取-液相色谱质谱/质谱法同时测定茶叶中吡虫啉、啶虫脒、茚虫威和氯虫苯甲酰胺农药残留的方法。方法样品经乙腈,无水硫酸镁提取,离心后取有机相以N-丙基乙二胺(PSA)和无水硫酸镁作为分散固相萃取试剂去除杂质,浓缩后以乙腈定容,液相色谱-质谱/质谱检测。对超声提取的温度和时间以及PSA用量进行了优化,获得了最佳的超声萃取条件,优化了质谱条件。结果 4种杀虫剂在0μg/L～200μg/L浓度内线性关系良好(r值为0.996 9～0.999 9),检出限为0.000 3 mg/kg,低、中、高3个加标水平下回收率分别为72.1%～82.6%、74.5%～85.2%、70.3%～83.1%,相对标准偏差(RSD)为0.6%～4.5%。结论该方法操作简便,试剂消耗量少,回收率稳定,结果准确,适合同时检测茶叶中吡虫啉、啶虫脒、茚虫威和氯虫苯甲酰胺农药残留。
Objective To establish a method for the simultaneous determination of imidacloprid, acetamiprid, indoxacarb and chlorantraniliprole pesticide residues in tea by dispersive solid-phase extraction(DSPE) and liquid chromatography tandem mass spectrometry(LC-MS/MS). Methods The samples were extracted with acetonitril and anhydrous magnesium sulfate. After centrifugation, the organic phase was purified with primary secondary amine(PSA) and anhydrous magnesium sulfate as the dispersive solid phase extraction reagent. After concentration, acetone was quantified by LC-MS/MS. The amounts of PSA, the temperature and the time of ultrasonic extraction were optimized to obtain the best ultrasonic extraction conditions. Furthermore, the conditions of mass spectrometry were optimized. Results The linear relationship for four kinds of pesticides was good within 0 μg/L-200 μg/L, and the correlation coefficient(r) was within 0.996 9-0.999 9. The detection limit was 0.000 3 mg/kg, the recoveries of three spiking levels were within 72.1%-82.6%, 74.5%-85.2% and 70.3%-83.1% respectively, and the relative standard deviation(RSD) was within 0.6%-4.5%. Conclusion The method is easy to operate, with less reagent consumption, stable recoveries, accurate and reliable results, which is suitable for simultaneous determination of imidacloprid, acetamiprid, indoxacarb and chlorantraniliprole pesticide residues in tea.
Objective To establish a method for the simultaneous determination of imidacloprid, acetamiprid, indoxacarb and chlorantraniliprole pesticide residues in tea by dispersive solid-phase extraction(DSPE) and liquid chromatography tandem mass spectrometry(LC-MS/MS). Methods The samples were extracted with acetonitril and anhydrous magnesium sulfate. After centrifugation, the organic phase was purified with primary secondary amine(PSA) and anhydrous magnesium sulfate as the dispersive solid phase extraction reagent. After concentration, acetone was quantified by LC-MS/MS. The amounts of PSA, the temperature and the time of ultrasonic extraction were optimized to obtain the best ultrasonic extraction conditions. Furthermore, the conditions of mass spectrometry were optimized. Results The linear relationship for four kinds of pesticides was good within 0 μg/L-200 μg/L, and the correlation coefficient(r) was within 0.996 9-0.999 9. The detection limit was 0.000 3 mg/kg, the recoveries of three spiking levels were within 72.1%-82.6%, 74.5%-85.2% and 70.3%-83.1% respectively, and the relative standard deviation(RSD) was within 0.6%-4.5%. Conclusion The method is easy to operate, with less reagent consumption, stable recoveries, accurate and reliable results, which is suitable for simultaneous determination of imidacloprid, acetamiprid, indoxacarb and chlorantraniliprole pesticide residues in tea.
引文
[1] 郑娣,叶延东,鲁芳.气相色谱-三重四级杆串联质谱法测定茶叶中茚虫威、溴虫腈、啶虫脒残留[J].食品安全质量检测学报,2016,7(12):4919-4924.
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[4] 许欣欣,王冰,陈慧玲,等.气相色谱-质谱联用法测定茶叶中溴虫腈、啶虫脒和茚虫威[J].预防医学情报杂志,2017,33(9):901-904.
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[6] 陈俊玉,何建顺,余晓薇,等.液相色谱-质谱法测定植物源食品中氯虫苯甲酰胺残留量[J].广州化工,2016,44(20):79-81.
[7] 成婧,王美玲,朱绍华,等.固相萃取-高效液相色谱-串联质谱法测定茶叶中啶虫脒、吡虫啉和氟虫腈残留量[J].食品安全质量检测学报,2016,7(1):131-137.
[8] 段兵,何太喜,范媛媛,等.凝胶渗透色谱-超高效液相色谱-串联质谱测定茶叶中吡虫啉和啶虫脒[J].食品科学,2016,37(4):238-241.
[9] 江泽军,石梦琪,刘广洋,等.液相色谱-串联质谱法测定21种植物源性食品中茚虫威残留[J].分析测试学报,2015,34(8):867-873.
[10] 路海燕,李斌,陈忠正,等.分散固相萃取-HPLC检测绿茶茶汤中吡虫啉和啶虫脒残留[J].食品科学,2013,34(20):203-206.
[11] 张新忠,罗逢健,陈宗懋,等.分散固相萃取净化超高效液相色谱串联质谱法研究茶叶与茶汤中茚虫威残留降解规律[J].分析测试学报,2013,32(1):1-8.
[12] 诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.
[13] 赵风年,石梦琪,李辉,等.分散固相萃取-液质联用法检测玉米中4种农药[J].食品研究与开发,2016,37(7):128-132.
[14] 郭虹,任武洁,魏玉霞,等.分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜中7种植物生长调节剂[J].中国卫生检验杂志,2018,28(6):660-663,666.
[15] 王颖,黄璐瑶,余晓琴,等.高效液相色谱-串联质谱法测定豆制品中3种甲基咪唑类化合物[J].中国卫生检验杂志,2018,28(4):415-418.
[16] 张力群,金铨,刘少颖,等.超高效液相色谱-串联质谱法同时检测环境水中5种苯二氮卓类镇静剂药物[J].中国卫生检验杂志,2018,28(2):142-145.
[2] 童小麟,陈建民.我国出口欧盟茶叶农药残留超标通报的分析与应对[J].检验检疫学刊,2015,25(1):16-18.
[3] 李晔,郭蒙京,袁佗.气相色谱-质谱法测定茶叶中溴虫腈、啶虫脒、茚虫威、三氯杀螨醇及拟除虫菊酯等11种农药残留[J].中国卫生检验杂志,2016,26(11):1579-1581,1584.
[4] 许欣欣,王冰,陈慧玲,等.气相色谱-质谱联用法测定茶叶中溴虫腈、啶虫脒和茚虫威[J].预防医学情报杂志,2017,33(9):901-904.
[5] 周华,张蕴,吴平谷,等.固相萃取-气相色谱质谱联用法测定茶叶中溴虫腈和茚虫威[J].卫生研究,2016,45(5):817-820.
[6] 陈俊玉,何建顺,余晓薇,等.液相色谱-质谱法测定植物源食品中氯虫苯甲酰胺残留量[J].广州化工,2016,44(20):79-81.
[7] 成婧,王美玲,朱绍华,等.固相萃取-高效液相色谱-串联质谱法测定茶叶中啶虫脒、吡虫啉和氟虫腈残留量[J].食品安全质量检测学报,2016,7(1):131-137.
[8] 段兵,何太喜,范媛媛,等.凝胶渗透色谱-超高效液相色谱-串联质谱测定茶叶中吡虫啉和啶虫脒[J].食品科学,2016,37(4):238-241.
[9] 江泽军,石梦琪,刘广洋,等.液相色谱-串联质谱法测定21种植物源性食品中茚虫威残留[J].分析测试学报,2015,34(8):867-873.
[10] 路海燕,李斌,陈忠正,等.分散固相萃取-HPLC检测绿茶茶汤中吡虫啉和啶虫脒残留[J].食品科学,2013,34(20):203-206.
[11] 张新忠,罗逢健,陈宗懋,等.分散固相萃取净化超高效液相色谱串联质谱法研究茶叶与茶汤中茚虫威残留降解规律[J].分析测试学报,2013,32(1):1-8.
[12] 诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.
[13] 赵风年,石梦琪,李辉,等.分散固相萃取-液质联用法检测玉米中4种农药[J].食品研究与开发,2016,37(7):128-132.
[14] 郭虹,任武洁,魏玉霞,等.分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜中7种植物生长调节剂[J].中国卫生检验杂志,2018,28(6):660-663,666.
[15] 王颖,黄璐瑶,余晓琴,等.高效液相色谱-串联质谱法测定豆制品中3种甲基咪唑类化合物[J].中国卫生检验杂志,2018,28(4):415-418.
[16] 张力群,金铨,刘少颖,等.超高效液相色谱-串联质谱法同时检测环境水中5种苯二氮卓类镇静剂药物[J].中国卫生检验杂志,2018,28(2):142-145.