Determination of organochlorine pesticide residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry

doi:10.3724/SP.J.1123.2015.10034

Abstract

Abstract:

A method was developed for the determination of 10 organochlorine pesticide (OCP) residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry (GC-NCI-TOF-MS) coupled with QuEChERS method. The extraction and purification procedures for tobacco samples, the chromatographic conditions and TOF-MS conditions of the analytes were critically examined. Tobacco samples were extracted with ethyl acetate-hexane (1 : 1, v/v) and cleaned up by primary secondary amine (PSA) and MgSO₄, then detected by GC-NCI-TOF-MS. Accurate mass analysis, isotopic peak clusters, fragment ion abundance ratio and retention time were employed to qualitative identification and external standard method was used for quantitative determination. The results indicated that the correlation coefficients (r²) were better than 0.997, and the relative standard deviations (RSDs) were less than 6.5%. The limits of detection and the limits of quantification were 0.04 to 0.80 μ g/kg and 0.13 to 2.64 μ g/kg, respectively. The recoveries of the 10 organochlorine pesticides at three spiked levels ranged from 77.2% to 93.0%. It was proved that the method is simple, rapid, with high accuracy and high sensitive. It is appropriate for the detection and determination of organochlorinepesticide residues in tobacco samples.

Key words: gas chromatography-negative chemical ionization-time of flight mass spectrometry (GC-NCI-TOF-MS), organochlorine pesticide (OCP), QuEChERS, tobacco

CLC Number:

O658

SI Xiaoxi, LU Sheming, LIU Zhihua, ZHU Li, LIU Chunbo, ZHANG Fengmei, HE Pei, ZHU Ruizhi. Determination of organochlorine pesticide residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(3): 340-345.

References

[1] Bempah C K, Archibold B K, Enimil E, et al. Food Control, 2012, 25(2): 537
[2] Dewan P, Jain V, Gupta P, et al. Chemosphere, 2013, 90(5): 1704
[3] Qi D W, Fei T, Sha Y F, et al. J Chromatogr A, 2014, 1374: 273
[4] Zhao J, Wang H, Chen Q D, et al. Chinese Journal of Analytical Chemistry, 2009, 37(3): 351 赵洁, 王恒, 陈庆东, 等. 分析化学, 2009, 37(3): 351
[5] Du J, Lü B, Zhu P, et al. Chinese Journal of Chromatography, 2013, 31(8): 739 杜娟, 吕冰, 朱盼, 等. 色谱, 2013, 31(8): 739
[6] Ghosh R K, Khan Z S, Rao C V N, et al. Environ Monit Assess, 2014, 186(8): 5069
[7] Wang Y, Zhu C H, Zou X L, et al. Chinese Journal of Chromatography, 2013, 31(11): 1076 王宇, 朱成华, 邹晓莉, 等. 色谱, 2013, 31(11): 1076
[8] YC/T 405.2-2011
[9] Zhang X, Mobley N, Zhang J G, et al. J Agric Food Chem, 2010, 58(22): 11553
[10] Rothweiler B, Berset J D. Chemosphere, 1999, 38(7): 1517
[11] Cao X Y, Pang G F, Jing L H, et al. Chinese Journal of Chromatography, 2015, 33(4): 389 曹新悦, 庞国芳, 金铃和, 等. 色谱, 2015, 33(4): 389
[12] Wu J L, Leung K F, Tong S F, et al. Rapid Commun Mass Spectrom, 2012, 26(2): 123
[13] Russo M V, Campanella L, Avino P. J Chromatogr B, 2002, 780(2): 431
[14] Shen C Y, Cao X W, Shen W J, et al. Talanta, 2011, 84(1): 141
[15] Kazda R, Hajšlová J, Poustka J, et al. Anal Chim Acta, 2004, 520(1/2): 237
[16] Lou X H, Gao C C, Zhu W J, et al. Chinese Tobacco Science, 2012, 33(5): 83 楼小华, 高川川, 朱文静, 等. 中国烟草科学, 2012, 33(5): 83
[17] Luo Y B, Li X, Jiang X Y, et al. J Chromatogr A, 2015, 1406: 1
[18] YC/T 31-1996
[19] Koesukwiwat U, Lehotay S J, Mastovska K, et al. J Agric Food Chem, 2010, 58 (10): 5950
[20] Leandro C C, Hancock P, Fussell R J, et al. J Chromatogr A, 2006, 1103: 94