气相色谱-飞行时间质谱快速鉴定和定量测定烟草中43种农药
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- 英文论文题名：Rapid Screening and Determination of 43 Pesticide Residues in Tobacco by Gas Chromatography- Time of Flight Mass Spectrometry
- 论文作者：司晓喜 ; 朱瑞芝 ; 刘志华 ; 马雪英 ; 朱丽 ; 张凤梅 ; 刘春波 ; 陆舍铭
- 英文论文作者：SI Xiao-xi ; ZHU Rui-zhi ; LIU Zhi-hua ; MA Xue-ying ; ZHU Li ; ZHANG Feng-mei ; LIU Chun-bo ; LU She-ming ; R&D Center of China Tobacco Yunnan Industrial Co. ; Ltd. ; Key Laboratory of Tobacco Chemistry of Yunnan ; Yunnan Tobacco Materials(group) Co. ; Ltd.
- 年：2016
- 作者机构：云南省烟草化学重点实验室云南中烟工业有限责任公司技术中心;云南中烟物资(集团)有限责任公司;
- 论文关键词：烟草 ; 农药 ; QuEChERs ; 电子轰击电离 ; 气相色谱 ; 飞行时间质谱
- 英文论文关键词：tobacco ; pesticide ; QuEChERS ; electron impact ionization ; gas chromatography ; TOF MS
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：中文
- 分类号：TS47;O657.63
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：7
- 文件大小：429k
- 原文格式：D
摘要
建立了烟草中43种农药的气相色谱-飞行时间质谱(GC-TOF MS)分析方法。采用改进的QuEChERS前处理方法,样品以丙酮-正己烷(1:1)进行萃取,萃取液经N-丙基乙二胺(PSA)吸附剂分散固相萃取净化后,用GC-NCI-TOF MS进行检测。通过高分辨飞行时间质谱的精确质量数测定,建立了农药的特征离子数据库,结合目标物保留时间、碎片离子的丰度比、裂解规律、同位素离子峰簇等进行目标物定性鉴定。配制基质匹配标准曲线,以磷酸三苯酯(TPP)为内标进行定量测定。43种农药的线性相关系数(r~2)均不小于0.993,相对标准偏差不大于9.6%,定量下限为1.3~5.0μg/kg;在3个水平下的加标回收率为76.4%~96.6%。该方法简单快速,准确性和灵敏度高,满足烟草中多农药残留的定性和定量检测要求。
A rapid and accurate method was developed for the analysis of 43 pesticide residues in tobacco based on gas chromatography- time of flight mass spectrometry(GC- TOF MS).By modified QuEChERS method,tobacco samples were extracted with acetone-hexane(1:1),and cleaned up with primary secondary amine(PSA),then detected by GC- TOF MS.Precise mass database of characteristic ions by TOF MS,coupled with retention time,fragment ion abundance ratios,fragmentation patterns of characteristic fragment ions,isotopic peak clusters were employed for the qualitative identification of pesticides.The quantatative method was established using the matrix-matched calibration standards with triphenyl phosphate(TPP) as the internal standard.The results indicated that the linear correlation coefficients(r~2) were not less than 0.993 with relative standard deviations(RSD) not more than 9.6%,and quantitation limits of 1.3-5.0μg/kg.The recoveries of 43 pesticides at three spiked concentration levels ranged from 76.4%to 96.6%.The method is simple,rapid,accurate and sensitive,and is appropriate for the determination of multi-residues in tobacco.
A rapid and accurate method was developed for the analysis of 43 pesticide residues in tobacco based on gas chromatography- time of flight mass spectrometry(GC- TOF MS).By modified QuEChERS method,tobacco samples were extracted with acetone-hexane(1:1),and cleaned up with primary secondary amine(PSA),then detected by GC- TOF MS.Precise mass database of characteristic ions by TOF MS,coupled with retention time,fragment ion abundance ratios,fragmentation patterns of characteristic fragment ions,isotopic peak clusters were employed for the qualitative identification of pesticides.The quantatative method was established using the matrix-matched calibration standards with triphenyl phosphate(TPP) as the internal standard.The results indicated that the linear correlation coefficients(r~2) were not less than 0.993 with relative standard deviations(RSD) not more than 9.6%,and quantitation limits of 1.3-5.0μg/kg.The recoveries of 43 pesticides at three spiked concentration levels ranged from 76.4%to 96.6%.The method is simple,rapid,accurate and sensitive,and is appropriate for the determination of multi-residues in tobacco.
引文
[1]Bempah C K,Buah-Kwofie A,Enimil E,Blewu B,Agyei-Martey G.Food Control,2012,25(2):537-542.
[2]Chen X S,Bian Z Y,Hou H W,Yang F,Liu S S,Tang G L,Hu Q Y.J.Agric.Food Chem.,2013,61(24):5746-5757.
[3]Dewan P,Jain V,Gupta P,Banerjee D B.Chemosphere,2013,90(5):1704-1710.
[4]Ghosh R K,Khan Z S,Rao C V N,Banerjee K,Reddy D D,Murthy T K G,Johnson N,Ray D P.Environ.Monit.Assess.,2014,186(8):5069-5075.
[5]Su J F,Zhong M S,Chen J,Guo X,Chen J X,Liang Z,Liu J J.J.Instrum.Anal.(苏建峰,钟茂生,陈晶,郭昕,陈劲星,梁震,刘建军.分析测试学报),2015,34(6):625-638.
[6]Fernandes V C,Vera J L,Domingues V F,Ailva L M S,Mateus N,Delerue-Matos C.J.Am.Soc.Mass Spectrom.,2012,23(12):2187-2197.
[7]Souza-Silva E A,Pawliszyn J.J.Agric.Food Chem.,2015,63(18):4464-4477.
[8]Banerjee K,Dasgupta S,Utture S C.Compr.Anal.Chem.,2012,58:367-413.
[9]Ma Z L,Li L Y,Liu X Y,Wei C B,Liu Y G,Liu S,Fang J.Chin.J.Trop.Crops(马智玲,李凌云,刘新艳,魏长宾,刘玉革,刘肃,方佳.热带作物学报),2015,36(4):804-812.
[10]Mastovska K,Dorweiler K J,Lehotay S J,Wegscheid J S,Szpylka K A.J.Agric.Food Chem.,2009,58(10):5959-5972.
[11]Cheng Q,Yang F,Li J,Lu S Y,Lan J C,Jiang J B.J.Instrum.Anal.(程权,杨方,李捷,卢声宇,蓝锦昌,江锦彬.分析测试学报),2015,34(5):525-531.
[12]Zhang L J,Liu S W,Cui X Y,Pan C P,Zhang A L,Chen F.Cent.Eur.J.Chem.,2012,10(3):900-925.
[13]Wang L Z,Huang X Y,Chen Y,Lin Z X,Wang G F,Zhou Y.J.Instrum.Anal.(王连珠,黄小燕,陈泳,林子旭,王根芳,周昱.分析测试学报),2014,33(10):1102-1108.
[14]Shen X L,Sun B L,Dong Y W,Yan Z H,Wang C H.Mod.Sci.Instrum.(申秀丽,孙宝利,董一威,闫忠会,汪聪慧.现代科学仪器),2009,(1):84-87.
[15]Ge N,Liu X M,LiXM,Huang X Z,Wu Y P,Li J,Liu Y M.J.Instrum.Anal.(葛娜,刘晓茂,李学民,黄学者,吴艳萍,李金,刘永明.分析测试学报),2011,30(12):1351-1355.
[16]Zhang X,Mobley N,Zhang J G,Zheng X M,Lu L,Ragin 0,Smith C J.J.Agric.Food Chem.,2010,58(22):11553-11560.
[17]Wu J,Leung K F,Tong S F,Lam C W.Rapid Commun.Mass Spectrom.,2012,26(2):123-132.
[2]Chen X S,Bian Z Y,Hou H W,Yang F,Liu S S,Tang G L,Hu Q Y.J.Agric.Food Chem.,2013,61(24):5746-5757.
[3]Dewan P,Jain V,Gupta P,Banerjee D B.Chemosphere,2013,90(5):1704-1710.
[4]Ghosh R K,Khan Z S,Rao C V N,Banerjee K,Reddy D D,Murthy T K G,Johnson N,Ray D P.Environ.Monit.Assess.,2014,186(8):5069-5075.
[5]Su J F,Zhong M S,Chen J,Guo X,Chen J X,Liang Z,Liu J J.J.Instrum.Anal.(苏建峰,钟茂生,陈晶,郭昕,陈劲星,梁震,刘建军.分析测试学报),2015,34(6):625-638.
[6]Fernandes V C,Vera J L,Domingues V F,Ailva L M S,Mateus N,Delerue-Matos C.J.Am.Soc.Mass Spectrom.,2012,23(12):2187-2197.
[7]Souza-Silva E A,Pawliszyn J.J.Agric.Food Chem.,2015,63(18):4464-4477.
[8]Banerjee K,Dasgupta S,Utture S C.Compr.Anal.Chem.,2012,58:367-413.
[9]Ma Z L,Li L Y,Liu X Y,Wei C B,Liu Y G,Liu S,Fang J.Chin.J.Trop.Crops(马智玲,李凌云,刘新艳,魏长宾,刘玉革,刘肃,方佳.热带作物学报),2015,36(4):804-812.
[10]Mastovska K,Dorweiler K J,Lehotay S J,Wegscheid J S,Szpylka K A.J.Agric.Food Chem.,2009,58(10):5959-5972.
[11]Cheng Q,Yang F,Li J,Lu S Y,Lan J C,Jiang J B.J.Instrum.Anal.(程权,杨方,李捷,卢声宇,蓝锦昌,江锦彬.分析测试学报),2015,34(5):525-531.
[12]Zhang L J,Liu S W,Cui X Y,Pan C P,Zhang A L,Chen F.Cent.Eur.J.Chem.,2012,10(3):900-925.
[13]Wang L Z,Huang X Y,Chen Y,Lin Z X,Wang G F,Zhou Y.J.Instrum.Anal.(王连珠,黄小燕,陈泳,林子旭,王根芳,周昱.分析测试学报),2014,33(10):1102-1108.
[14]Shen X L,Sun B L,Dong Y W,Yan Z H,Wang C H.Mod.Sci.Instrum.(申秀丽,孙宝利,董一威,闫忠会,汪聪慧.现代科学仪器),2009,(1):84-87.
[15]Ge N,Liu X M,LiXM,Huang X Z,Wu Y P,Li J,Liu Y M.J.Instrum.Anal.(葛娜,刘晓茂,李学民,黄学者,吴艳萍,李金,刘永明.分析测试学报),2011,30(12):1351-1355.
[16]Zhang X,Mobley N,Zhang J G,Zheng X M,Lu L,Ragin 0,Smith C J.J.Agric.Food Chem.,2010,58(22):11553-11560.
[17]Wu J,Leung K F,Tong S F,Lam C W.Rapid Commun.Mass Spectrom.,2012,26(2):123-132.
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