Determination of 34 pesticide residues in rice, proso millet and wheat with QuEChERS-on line gel permeation chromatography-gas chromatography-mass spectrometry

doi:10.3724/SP.J.1123.2013.07029

Abstract

Abstract:

A method for the simultaneous determination of 34 pesticides in rice, proso millet and wheat by QuEChERS coupled with on line gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS) was developed. The effects of the sample weight, extraction solvent, sorbent for purification were investigated. The matrix effect and the usefulness of analyte protectant were also studied. The identification and quantification were performed by GPC-GC-MS in selected ion monitoring (SIM) mode and external standard method. The calibration curves of the 34 pesticides showed good linearity in the range of 0.0125-0.2 mg/L with the correlation coefficients (r²) between 0.968 and 0.999. The average recoveries were 94.5%-117.1%, 83.1%-121.7% and 93.1%-120.2% with the relative standard deviations (RSDs, n=6) no more than 14.5%, 15.1% and 15.2% in rice, proso millet and wheat samples, respectively. The LODs of this method were 0.0281-5.31, 0.0282-4.82 and 0.0273-5.13 μg/kg (S/N=3) for rice, proso millet and wheat samples, respectively. The low cost and less consumption of reagents of this method are in accordance with the concept of green chemistry. The convenient operation and versatility of this method are suitable for the fast screening and detection of the 34 pesticide residues in rice, proso millet and wheat.

Key words: fast screening, gel permeation chromatography-gas chromatography-mass spectrometry (GPC-GC-MS), pesticide residues, QuEChERS

CLC Number:

O658

RUAN Hua, RONG Weiguang, MA Yongjian, JI Wenliang, LIU Hualiang, SONG Ninghui. Determination of 34 pesticide residues in rice, proso millet and wheat with QuEChERS-on line gel permeation chromatography-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(12): 1211-1217.

References

[1] Xu D M, Lu S Y, Chen D J, et al. Chinese Journal of Chromatography (徐敦明, 卢声宇, 陈达捷, 等. 色谱), 2013, 31(3): 218
[2] Chen H P, Liu X, Wang Q H, et al. Chinese Journal of Chromatography (陈红平, 刘新, 汪庆华, 等. 色谱), 2011, 29(5): 409
[3] Tian S Q, Mao X H, Miao S, et al. Chinese Journal of Chromatography (田绍琼, 毛秀红, 苗水, 等. 色谱), 2012, 30(1): 14
[4] Han X, Lou X S, Zhang L, et al. Chinese Journal of Chromatography (韩笑, 娄喜山, 张莉, 等. 色谱), 2010, 28(4): 341
[5] Cappelini L T D, Cordeiro D, Brondi S H G, et al. Environ Technol, 2012, 33(20): 2299
[6] Tankiewicz M, Morrison C, Biziuk M. Talanta, 2013, 107: 1
[7] Wilkowska A, Biziuk M. Food Chem, 2011, 125(3): 803
[8] Lu D S, Qiu X L, Feng C, et al. J Chromatogr B, 2012, 895: 17
[9] Diez C, Traag W A, Zommer P, et al. J Chromatogr A, 2006, 1131: 11
[10] Wang L Z, Zhou Y, Chen Y, et al. Chinese Journal of Chromatography (王连珠, 周昱, 陈泳, 等. 色谱), 2012, 30(2): 146
[11] 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
[12] Shi Z H, Zhang X Y, Bu S J, et al. Chinese Journal of Chromatography (施祖灏, 张小燕, 卜士金, 等. 色谱), 2012, 30(9): 883
[13] Liu Y W, Dong Y W, Sun B L, et al. Food Science (刘亚伟, 董一威, 孙宝利, 等. 食品科学), 2009, 30(9): 285
[14] Liu M M, Kang S, Yao C. Chinese Journal of Pesticide Science (刘满满, 康澍, 姚成. 农药学学报), 2013, 15(1): 8
[15] Hercegova A, Domotorová M, Kruzlicová D, et al. J Sep Sci, 2006, 29(8): 1102
[16] Lu D S, Xiong L B, Wen Y M, et al. Journal of Chinese Mass Spectrometry Society (卢大胜, 熊丽蓓, 温忆敏, 等. 质谱学报), 2011, 32(4): 229
[17] Schenzler C, Thier H P. Food Addit Contam, 2001, 18(10): 875
[18] Ministry of Health, Labor and Welfare of Japan. Analytical Methods for Residual Compositional Substances of Agricultural Chemicals, Feed Additives, and Veterinary Drugs in Food. 2006
[19] Environmental Protection Agency (EPA). Method 3640A Gel-Permeation Cleanup. Version 1, 1994
[20] GB/T 19650-2006
[21] Li Y, Cai Y, Yang S Q, et al. Chinese Journal of Health Laboratory Technology (李琰, 蔡跃, 杨胜琴, 等. 中国卫生检验杂志), 2011, 21(2): 277
[22] Hui E J, Sheng Z H, Fang W Z, et al. Chinese Journal of Experimental Traditional Medical Formulae (惠恩健, 盛振华, 方文忠, 等. 中国实验方剂学杂志), 2013, 19(8): 138
[23] Sheng Z H, Wu J J, Lu L, et al. Chinese Archives of Traditional Chinese Medicine (盛振华, 吴君金, 卢林, 等. 中华中医药学刊), 2011, 29(8): 1856
[24] Jia W, Ling Y, Hao J, et al. Journal of Instrumental Analysis (贾玮, 凌云, 郝静, 等. 分析测试学报), 2012, 31(10): 1217
[25] Hu B Z, Song W H, Dong W H, et al. Advanced Measurement and Laboratory Management (胡贝贞, 宋伟华, 董文洪, 等. 现代测量与实验室管理), 2012(1): 29
[26] State Quality and Technical Supervision. JJF1059-1999 China National Metrology Technical Specifications: Evaluation and Expression of Uncertainty in Measurement (国家质量技术监督局. JJF1059-1999中华人民共和国国家计量技术规范: 测量不确定度评定与表示), 1999
[27] Yang X, Zhang H, Liu Y, et al. Food Chem, 2011, 127(2): 855
[28] Deutsche Forschungsgemeinschaft (DFG). Manual of Pesticide Residue Analysis, Method S19. Weinheim, Germany: VCH, 1999
[29] Lee S M, Papathakis M L, Feng H M C, et al. Fresenius J Anal Chem, 1991, 339(6): 376
[30] Hou X, Han M, Dai X H, et al. Food Chem, 2013, 138: 1198
[31] Mastovska K, Dorweiler K J, Lehotay S J, et al. J Agric Food Chem, 2010, 58(10): 5959
[32] Koesukwiwat U, Sanguankaew K, Leepipatpiboon N. Anal Chim Acta, 2008, 626(1): 10
[33] Fenik J, Tankiewicz M, Biziuk M. TrAC, Trends Anal Chem, 2011, 30(6): 814
[34] Poole C F. J Chromatogr A, 2007, 1158: 241
[35] Lehotay S J, Schaner A, Nemoto S, et al. J AOAC Int, 2002, 85(5): 1148
[36] Wang Y, Jin H Y, Ma S C, et al. J Chromatogr A, 2011, 1218(2): 334
[37] European Commission. Regulation (EC) No. 396/2005 of the European Parliament and of the Council of 23 February 2005 on Maximum Residue Levels of Pesticides in or on Food and Feed of Plant and Animal Origin and Amending Council Directive 91/414/EEC. [2013-10-18]. http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L: 2005: 070: 0001: 0016:en:PDF
[38] European Commission. Document No. SANCO/12495/2011. Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed. [2013-11-07]. http://ec.europa.eu/food/plant/plant_protection_products/guidance_documents/docs/qualcontrol_en.pdf