PDF《气相色谱 -串联质谱技术分析烟草中的 132 种农药残留》

2012 年10 月Vol.

30 No.

10 October

2012 Chinese Journal of Chromatography

1043 ~

1055 研究论文 DOI: 10.

3724 / SP. J. 1123. 2012.

06031 ?通讯联系人:唐纲岭,硕士,高级工程师,主要从事烟草化学、烟草质量检验研究. Tel: (0371)67672613, E-mail: tglcttc@ 163. com. 胡清源,博士,研究员,主要从事烟草化学、烟草质量检验研究. Tel: (0371)67672601, E-mail: huqy@ ztri. com. cn. 基金项目:国家烟草专卖局标准项目(502011AB0450)和中国烟草总公司郑州烟草研究院院长基金项目(512012CA0080). 收稿日期:2012-06-21 气相色谱-串联质谱技术分析烟草中的

132 种农药残留 陈晓水, 边照阳, 唐纲岭? , 胡清源? (国家烟草质量监督检验中心, 河南 郑州 450001) 摘要:利用气相色谱-串联质谱(GC-MS/ MS)检测技术,建立了检测烟草中的

132 种农药残留的高灵敏度方法. 分 析过程中考察了不同萃取溶剂、不同缓冲盐体系、不同净化剂对目标物回收率的影响. 最终确定烟草样品以乙腈 进行提取,以N-丙基乙二胺(PSA)与碳 18(C18E)的混合净化剂进行净化,氮气吹近干后用正己烷-丙酮(9∶ 1, v/ v)复溶,过有机滤膜后进行 GC-MS/ MS 测定,内标法定量.

132 种农药在

20 ~

2 000 μg/ kg 之间线性关系良好(r2 >

0. 99);

所有农药的方法定量限(LOQ, S/ N = 10)均低于

20 μg/ kg;

在

50、

200、500 μg/ kg 的加标水平下,除灭蚁 灵及六氯苯回收率稍低外,其他农药的平均回收率为 68. 10% ~ 123. 15%,相对标准偏差(RSD)为1. 79% ~ 19. 88%. 对国际烟草科学研究合作中心(CORESTA)2012 年共同实验的烟草样品进行检测,对比本方法与已有的标准方法, 其结果一致性较好. 该方法准确、可靠,灵敏度好,适用于烟草中

132 种农药残留的快速筛查与定性、定量分析. 关键词:气相色谱-串联质谱;

多农药残留;

烟草 中图分类号:O658 文献标识码:A 文章编号:1000-8713(2012)10-1043-13 Determination of

132 pesticide residues in tobacco by gas chromatography-tandem mass spectrometry CHEN Xiaoshui, BIAN Zhaoyang, TANG Gangling? , HU Qingyuan? (China National Tobacco Quality Supervision and Test Center, Zhengzhou 450001, China) Abstract: A simple method for the determination of

132 pesticide residues in tobacco by gas chromatography-triple quadrupole tandem mass spectrometry ( GC-MS/ MS) was established. The influences of different extraction solvents, different buffer systems and different purifying agents on the recoveries of pesticides were investigated. The tobacco sample was extracted with acetonitrile, then cleaned up by the mixed sorbents of primary secondary amine ( PSA) and octadecylsilane ( C18E). After dried by nitrogen, the extract residue was reconstituted with n-hexane-acetone (9∶ 1, v / v). GC-MS/ MS in multi-reaction monitoring (MRM) mode was used as the detection method and triphenyl phosphate (TPP) as the internal standard. All of the

132 pesticides had good linear relationships (r2 >

0. 99) between

20 μg / kg and

2 000 μg / kg. At the three spiked levels of 50,

200 and

500 μg / kg in the tobacco extract, the average recover- ies of all the pesticides were in the range of 68. 10% to 123. 15% except for mirex and hexa- chlorobenzene;

moreover, the relative standard deviations ( RSDs) of them were between 1. 79% and 19. 88%. We participated in the CORESTA ( Cooperation Centre for Scientific Research Relative to Tobacco) 2012'

s co-experiment. The results of our method and the exis- ted standard methods had good consistency. The accurate, reliable and sensitive method can be applied to the determination of the