QuEChERS-液相色谱/高分辨质谱技术分析茶叶中农药残留
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摘要
建立液相色谱-四级杆飞行时间串联质谱技术检测茶叶中18种农药(久效磷、敌百虫、磷胺、对氧磷、杀扑磷、嘧菌酯、腈菌唑、三唑磷、丙线磷、苯线磷、杀虫畏、稻丰散、毒虫畏、丙环唑、异丙胺磷、吡唑硫磷、伏杀磷、丙烯菊酯)残留的方法.大部分物质在28 min内实现基线分离,结合精确质量数和保留时间信息,能将各组分准确定性.在最优的色谱-质谱条件下,待测物在2～1 000 ng·mL~(-1)范围内线性关系良好,检测限介于0.50～8.00 ng·mL~(-1)之间.采用快速样品前处理技术(QuEChERS)快速提取茶粉,各种样品的加标回收率均大于84.2%.方法具有灵敏度高、回收率好、检测简便等优点,能够满足茶叶中多种类农残快速分析的要求.
Simultaneous analysis of 18 kinds of pesticides(monocrotophos, trichlorfon, phosphamidon, paraoxon, methidathion, azoxystrobin, myclobutanil, triazophos, ethoprophos, fenamiphos, tetrachlorvinphos, phenthoate, chlorfenvinphos, propiconazole, isofenphos, pyraclofos, phosalone, allethrin) was established by liquid chromatography-quadrupole time-of-flight mass spectrometry. Most compounds were baseline separated in 28 min. Qualitative analysis of this method is excellent with accurate mass and retention time. Under the optimal conditions, good linear range in 2 to 1 000 ng·mL~(-1) was obtained, with the limit of detection between 0.50 to 8.00 ng·mL~(-1). QuEChERS method was used for rapid extraction and clean-up of tea sample. The recoveries of all tea samples were larger than 84.2%. The developed method was sensitive, rapid with good recovery, which can meet the fast determination demand of pesticide multi-residues in the tea.
Simultaneous analysis of 18 kinds of pesticides(monocrotophos, trichlorfon, phosphamidon, paraoxon, methidathion, azoxystrobin, myclobutanil, triazophos, ethoprophos, fenamiphos, tetrachlorvinphos, phenthoate, chlorfenvinphos, propiconazole, isofenphos, pyraclofos, phosalone, allethrin) was established by liquid chromatography-quadrupole time-of-flight mass spectrometry. Most compounds were baseline separated in 28 min. Qualitative analysis of this method is excellent with accurate mass and retention time. Under the optimal conditions, good linear range in 2 to 1 000 ng·mL~(-1) was obtained, with the limit of detection between 0.50 to 8.00 ng·mL~(-1). QuEChERS method was used for rapid extraction and clean-up of tea sample. The recoveries of all tea samples were larger than 84.2%. The developed method was sensitive, rapid with good recovery, which can meet the fast determination demand of pesticide multi-residues in the tea.
引文
[1] 中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局,农业部.食品安全国家标准食品中农药最大残留限量:GB 2763—2016[S].北京:中国标准出版社,2016.
[2] ANASTASSIADES M,LEHOTAY S J,?TAJNBAHER D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[3] 中华人民共和国农业部,国家食品药品监督管理总局,国家卫生和计划生育委员会.食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法:GB 23200.13—2016[S].北京:中国标准出版社,2016.
[4] 张桂云,杨伟强,林常青,等.分散固相萃取-超高效液相色谱串联质谱法测定茶叶中的7种农药残留[J].福州大学学报(自然科学版),2016,44(6):896-900.
[5] CHEN H P,GAO G W,CHAI Y F,et al.Multiresidue method for the rapid determination of pesticide residues in tea using ultra performance liquid chromatography orbitrap high resolution mass spectrometry and in-syringe dispersive solid phase extraction[J].ACS Omega,2017,2(9):5917-5927.
[6] WONG J W,WANG J,CHOW W C R,et al.Perspectives on liquid chromatography-high resolution mass spectrometry for pesticide screening in foods[J].Journal of Agricultural and Food Chemistry,2018,66(37):9573-9581.
[7] 周秀锦,陈宇,杨赛军,等.超高效液相色谱-四极杆飞行时间质谱法非靶向快速筛查进口粮谷中未知的农药残留[J].色谱,2017,35(8):787-793.
[8] 张建莹,罗耀,宫本宁,等.液相色谱-四极杆-飞行时间质谱法快速筛查苹果与生菜中248 种农药残留[J].分析测试学报,2018,37(2):154-164.
[9] 李春艳,孔祥虹,何强,等.改进的QuEChERS-GC-MS 法快速分析茶叶中30种农药残留[J].中国食物与营养,2010(2):57-60.
[2] ANASTASSIADES M,LEHOTAY S J,?TAJNBAHER D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[3] 中华人民共和国农业部,国家食品药品监督管理总局,国家卫生和计划生育委员会.食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法:GB 23200.13—2016[S].北京:中国标准出版社,2016.
[4] 张桂云,杨伟强,林常青,等.分散固相萃取-超高效液相色谱串联质谱法测定茶叶中的7种农药残留[J].福州大学学报(自然科学版),2016,44(6):896-900.
[5] CHEN H P,GAO G W,CHAI Y F,et al.Multiresidue method for the rapid determination of pesticide residues in tea using ultra performance liquid chromatography orbitrap high resolution mass spectrometry and in-syringe dispersive solid phase extraction[J].ACS Omega,2017,2(9):5917-5927.
[6] WONG J W,WANG J,CHOW W C R,et al.Perspectives on liquid chromatography-high resolution mass spectrometry for pesticide screening in foods[J].Journal of Agricultural and Food Chemistry,2018,66(37):9573-9581.
[7] 周秀锦,陈宇,杨赛军,等.超高效液相色谱-四极杆飞行时间质谱法非靶向快速筛查进口粮谷中未知的农药残留[J].色谱,2017,35(8):787-793.
[8] 张建莹,罗耀,宫本宁,等.液相色谱-四极杆-飞行时间质谱法快速筛查苹果与生菜中248 种农药残留[J].分析测试学报,2018,37(2):154-164.
[9] 李春艳,孔祥虹,何强,等.改进的QuEChERS-GC-MS 法快速分析茶叶中30种农药残留[J].中国食物与营养,2010(2):57-60.