账户: 密码:
气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留
详细信息    查看全文 | 推荐本文 | 收藏本文
  • 英文篇名:Identification of pesticide residues in common fruits and vegetables by gas chromatography-quadrupole time-of-flight mass spectrometry
  • 作者:李晓颍 ; 张红医 ; 常巧英 ; 范春林 ; 庞国芳 ; 曹喆 ; 王雯雯
  • 英文作者:LI Xiaoying;ZHANG Hongyi;CHANG Qiaoying;FAN Chunlin;PANG Guofang;CAO Zhe;WANG Wenwen;College of Chemistry and Environmental Science,Hebei University;Chinese Academy of Inspection and Quarantine;Agilent Technologies;
  • 关键词:气相色谱-四极杆飞行时间质谱 ; 农药残留 ; 常见水果 ; 常见蔬菜
  • 英文关键词:gas chromatography-quadrupole time-of-flight mass spectrometry(GC-QTOF MS);;pesticide residues;;common fruits;;common vegetables
  • 中文刊名:色谱
  • 英文刊名:Chinese Journal of Chromatography
  • 机构:河北大学化学与环境科学学院;中国检验检疫科学研究院;安捷伦科技有限公司;
  • 出版日期:2014-03-08
  • 出版单位:色谱
  • 年:2014
  • 期:03
  • 基金:“十二五”国家科技支撑计划项目(2012BAD29B01)
  • 语种:中文;
  • 页:68-77
  • 页数:10
  • CN:21-1185/O6
  • ISSN:1000-8713
  • 分类号:TS255.7;O657.63
摘要
建立了一种新型农药多残留检测方法。采用气相色谱-四极杆飞行时间质谱(GC-QTOF MS)结合Carbon NH2柱固相萃取净化可对不同类别的152种农药残留进行准确的鉴定。一级(MS1)精确质量数据库评价3~5个特征离子,以3个及以上特征离子检出且离子丰度比(Q/qi)合适作为一级质谱定性依据。对部分特征离子数不足及特征离子检出情况不符合条件的农药进行二级(MS2)确证,应用二级谱图库检索及镜像结果对比分析实现疑似农药确证。本文对梨、甘蓝、番茄3种代表性果蔬在5.0和10.0μg/kg 2个添加水平的152种农药进行测定,回收率在70%~120%范围的比例分别为甘蓝91.45%、94.08%,番茄88.20%、88.80%,梨86.84%、92.10%。本方法为常见果蔬中农药残留的准确判断提供了可靠依据,扩大了分析范围。
        A new screening method was developed for the determination of 152 pesticide multi-residues in different chemical species with a Carbon NH2column using solid-phase extraction(SPE)coupled with gas chromatography-quadrupole time-of-flight mass spectrometry(GC-QTOF MS).In the first stage(MS1) accurate mass database,up to three-five ions of the pesticides were monitored.The presence of at least three ions and the accomplishment of the intensity ratio(Q/qi)within the established tolerances were used as the confirmation of intensity criteria.The pesticides which have less characteristic ions or the peaks of the characteristic ions detected were up the tolerance were determined in the second stage(MS2) and the spectral difference was evaluated using MS2 library for the identified. Cabbage,tomato,pear were selected as typical fruits and vegetables to spike and detected all the 152 pesticides at two concentration levels of 5.0 and 10.0μg/kg.The recoveries in the range of 70%-120% at two concentration levels were 91.45% and 94.08% for cabbage,88.20% and 88.80% for tomato,86.84%and92.10% for pear respectively.Using the established 152 pesticide MS2 library some suspected pesticides were identified,and at the same time the analysis scope was expanded.
引文
[1]Xu P J,Gao X S,Tao B,et al.Chinese Journal of Analytical Chemistry(许鹏军,高晓莎,陶晡,等.分析化学),2008,36(11):1515
    [2]Wang L,Jin F,Li M J,et al.Chinese Journal of Analytical Chemistry(王丽,金芬,李敏洁,等.分析化学),2013,41(6):869
    [3]Shi J W,Li J G,Wang Y F,et al.Chinese Journal of Chromatography(施家威,李继革,王玉飞,等.色谱),2012,30(6):602
    [4]Shen W J,Yu K Y,Gui Q W,et al.Chinese Journal of Chromatography(沈伟健,余可垚,桂茜雯,等.色谱),2009,27(4):391
    [5]Wang J,Wang X,Liang X C,et al.Chinese Journal of Health Laboratory Technology(王江,王辛,梁晓聪,等.中国卫生检验杂志),2008,8(2):255
    [6]Li J G,Wang Y F,Shi J W,et al.Chinese Journal of Chromatography(李继革,王玉飞,施家威,等.色谱),2012,30(3):262
    [7]Ding M,Zhong D L,Tang F B,et al.Chinese Journal of Chromatography(丁明,钟冬莲,汤富彬,等.色谱),2013,31(2):117
    [8]Wang Y,Liu S B,Xie C M,et al.Chinese Journal of Analytical Chemistry(王耀,刘少彬,谢翠美,等.分析化学),2011,39(1):67
    [9]Ruan H,Rong W G,Ma Y J,et al.Chinese Journal of Chromatography(阮华,荣维广,马永建,等.色谱),2013,31(12):1211
    [10]Omar N,Bakar J,Muhammad K.Food Control,2013,34(2):318
    [11]Wang L Z,Zhou Y,Huang X Y,et al.Chinese Journal of Chromatography(王连珠,周昱,黄小燕,等.色谱),2013,31(12):1167
    [12]Ma Z L,Zhao W,Li L Y,et al.Chinese Journal of Chromatography(马智玲,赵文,李凌云,等.色谱),2013,31(3):228
    [13]Zhao Y,Liu Y,Jin Y,et al.Chinese Journal of Analysis Laboratory(赵颖,刘瑜,金雁,等.分析试验室),2011,30(12):59
    [14]Cui S H,Chen W S,Qian J L,et al.Chinese Journal of Chromatography(崔淑华,陈慰双,钱家亮,等.色谱),2013,31(9):885
    [15]Chen S A.Fujian Analysis&Testing(陈师安.福建分析测试),2012,21(1):8
    [16]Zhu Y Z,Feng Y N,Jin Z H.Chinese Journal of Chromatography(朱永哲,冯雅男,金正汉.色谱),2013,31(9):850
    [17]Hernández F,Portolés T,Pitarch E,et al.J Mass Spectrom,2009,44(1):1
    [18]Hernandez F,Portolés T,Pitarch E,et al.Anal Chem,2007,79(24):9494
    [19]Ibanez M,Sancho J V,McMillan D,et al.Trends Anal Chem,2008,27(5):481
    [20]Cervera M I,Portolés T,Pitarch E,et al.J Chromatogr A,2012,1244(1/2):168
    [21]Cǎjka T,HajslováJ.J Chromatogr A,2004,1058(1/2):251
    [22]Portolés T,Pitarch E,López F J,et al.J Chromatogr A,2011,1218(1/2):303
    [23]Zhao Z Y,Shi Z H,Kang J,et al.Chinese Journal of Chromatography(赵志远,石志红,康健,等.色谱),2013,31(4):372
    [24]Liu J J,Gong P,Zhang X M,et al.Chinese Journal of Chromatography(刘靖靖,宫萍,张晓梅,等.色谱),2012,30(10):1012
    [25]Gao F D,Zhao Y,Shao B,et al.Chinese Journal of Chromatography(高馥蝶,赵妍,邵兵,等.色谱),2012,30(6):560
    [26]Kim Y H,Kim K H.Anal Chim Acta,2013,780:46
    [27]European Commission Decision 2002/657/EC
    [28]Portolés T,Sancho J V,Hernández F,et al.J Mass Spectrom,2010,45(8):926
    [29]Canellas E,Vera P,Domeno C,et al.J Chromatogr A,2012,1235(1/2):141
    [30]Zhang F,Yu C T,Wang W W,et al.Anal Chim Acta,2012,757:39
    [31]Cristiana C L,Peter H,Richard J F,et al.J Chromatogr A,2007,1166(1/2):152
    [32]European Commission.Guidance Document on Residue Analytical Methods(SANCO/825/00/rev.8.1).(2010-11-16).http://www.crl-pesticides.eu

© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号

地址:北京市海淀区学院路29号 邮编:100083

电话:办公室:(+86 10)66554848;文献借阅:66554900、66554949;咨询服务:66554800;科技查新:66554700