A rapid method was developed for the determination of 22 pesticides in rice wine. The procedure involved an extraction with acetonitrile and a cleanup step using dispersive solid-phase extraction (d-SPE), and primary-secondary amine (PSA) and octadecylsilane (ODS) were used as sorbents. D-SPE had some advantages over some traditional prepara- tions, especially in time and cost. Both the extraction and cleanup only cost about 15 min per a sample. Then the GC-MS was used for quantitative and qualitative analysis. Matrix-matched standards solution and analyte protectant were compared to decrease the matrix effect, and the former showed a better efficacy. Acceptable linearity was achieved in the range of 0.05 - 0.30 mg/L. After matrix-matched standards calibration, recoveries were between 60 and 140%. For the most of pesticides, precision and repeatability were less than 10% and 16%, respectively. The result indicated that the developed method was suitable for the determination of the multi-pesticides in rice wine.
Keywordsd-SPERice WinePesticideGC-MSMatrix Effect
H. Yu, Y. Ying, X. Fu and H. Lu, “Quality Determination of Chinese Rice Wine Based on Fourier Transform Near Infrared Spectroscopy,” Journal of Near Infrared Spec- troscopy, Vol. 14, No. 1, 200, pp. 37-44. doi:10.1255/jnirs.584
D. T. Likas, N. G. Tsiropoulos and G. E. Miliadis, “Rapid Gas Chromatographic Method for the Determination of Famoxadone, Trifloxystrobin and Fenhexamid Residues in Tomato, Grape and Wine Samples,” Journal of Chro- matography A, Vol. 1150, No. 1-2, 2007, pp. 208-214. doi:10.1016/j.chroma.2006.08.041
A. Economou, H. Bo-titsi, S. Antoniou and D. Tsipi, “De- termination of Multi-class Pesticides in Wines by Solid- phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry,” Journal of Chromatography A, Vol. 1216, No. 31, 2009, pp. 5856-5867. doi:10.1016/j.chroma.2009.06.031
J. J. Jimenez, J. L. Bernal, M. J. Del Nozal, L. Toribio and J. Bernal, “Use of SPE—GC/EIMS for Residue Ana- lysis in Wine Elaborated from Musts Spiked with Formu- lations of Chlorpyri-phos—Methyl, Methiocarb, Dicofol, and Cyproconazol,” Journal of Separation Science, Vol. 30, No. 4, 2007, pp. 547-556. doi: 10.1002/jssc.200600345
I. Carpinteiro, M. Ramil, I. Rodríguez and R. Cela, “Determination of Fungicides in Wine by Mixed-mode Solid Phase Extraction and Liquid Chromatography Coupled to Tandem Mass Spectrometry,” Journal of Chromatography A, Vol. 1217, No. 48, 2010, pp. 7484-7492. doi:10.1016/j.chroma.2010.09.080
G. F. Pang, C. L. Fan, Y. M. Liu, Y. Z. Cao, J. J. Zhang, B. L. Fu, X. M. Li, Z. Y. Li and Y. P. Wu, “Multi-Resi- due Method for the Determination of 450 Pesticide Resi- dues in Honey, Fruit Juice and Wine by Double-Cartridge Solid-Phase Extraction/Gas Chromatogra-phy-Mass Spectrometry and Liquid Chromatography-Tandem Mass Spec- trometry,” Food Additives & Contaminants: Part A, Vol. 23, No. 8, 2006, pp. 777-810. doi:10.1080/02652030600657997
D. Zhan, R. E. Anli, N. Vural and M. Bayram, “Determination of Chloroanisoles and Chlorophenols in Cork and Wine by Using HS-SPME and GC-ECD Detection,” Jour- nal of the Institute of Brewing, Vol. 115, No. 1, 2009, pp. 71-77.
L. M. Ravelo-Pérez, J. Hernández-Borges, T. M. Borges- Miquel and Má Rodríguez-Delgado, “Solid-Phase Mi- croextraction and Sample Stacking Micellar Electroki- netic Chromatography for the Analysis of Pesticide Re- sidues in Red Wines,” Food Chemistry, Vol. 111, No. 3, 2008, pp. 764-770. doi:10.1016/j.foodchem.2008.04.020
M. Anastassiades, S. J. Lehotay, D. Tajnbaher and F. J. Schenck, “Fast and Easy Multiresidue Method Employing Acetonitrile Extrac-tion/Partitioning and ‘Dispersive Solid- Phase Extraction’ for the Determination of Pesticide Re- sidues in Produce,” Journal of AOAC International, Vol. 86, No. 2, 2003, pp. 412-431.
J. Dong, X. M. Gong, L. Zhang and H. T. Wang, “Determination of Imidacloprid, Tebufenozide, Avennectins and Hexythiazox in Vegetables by QuEChERS-HPLC,” Chi- nese Journal of Analysis Laboratory, Vol. 3, 2008, pp. 91-94.
S. H. Patil, K. Banerjee, S. Dasgupta, D. P. Oulkar, S. B. Patil, M. R. Jadhav, R. H. Savant, P. G. Adsule and M. B. Deshmukh, “Multiresidue Analysis of 83 Pesticides and 12 Dioxin-like Polychlorinated Biphenyls in Wine by Gas Chro-matography-Time-of-Flight Mass Spectrometry,” Jour- nal of Chromatography A, Vol. 1216, No. 12, 2009, pp. 2307-2319. doi:10.1016/j.chroma.2009.01.091
K. Zhang, J. W. Wong, D. G. Hayward, P. Sheladia, A. J. Krynitsky, F. J. Schenck, M. G. Webster, J. A. Ammann and S. E. Ebeler, “Multiresidue Pesticide Analysis of Wines by Dispersive Solid-Phase Extrac-tion and Ultra- high-Performance Liquid Chromatogra-phy-Tandem Mass Spectrometry,” Journal of Agricultural and Food Chem- istry, Vol. 57, No. 10, 2009, pp. 4019-4029. doi:10.1021/jf9000023
S. C. Cunha, J. O. Fernandes, A. Alves and M. Oliveira, “Fast Low-pressure Gas Chromatogra-phy-Mass Spectro- metry Method for the Determination of Multiple Pesti- cides in Grapes, Musts and Wines,” Journal of Chroma- tography A, Vol. 1216, No. 1, 2009, pp. 119-126. doi:10.1016/j.chroma.2008.11.015
X. Xu, L. Li, W. Zhong and Y. He, “Rapid GC-MS Ana- lysis of Pesticide Residues Using Analyte Protectants,” Analytical Letters, Vol. 42, No. 16, 2009, pp. 2578-2591. doi:10.1080/00032710903243646
J. M. Lee, J. W. Park, G. C. Jang and K. J. Hwang, “Com- parative Study of Pesticide Multi-Residue Extraction in Tobacco for Gas Chromatogra-phy—Triple Quadrupole Mass Spectrometry,” Journal of Chromatography A, Vol. 1187, No. 1, 2008, pp. 25-33. doi:10.1016/j.chroma.2008.02.035
Y. Jiang, X. Li, J. Xu, C. Pan, J. Zhang and W. Niu, “Multiresidue Method for the Determination of 77 Pes- ticides in Wine Using QuEChERS Sample Preparation and Gas Chromatography with Mass Spec-trometry,” Food Additives & Contaminants: Part A, Vol. 26, No. 6, 2009, pp. 859-866. doi:10.1080/02652030902822794
W. Shen, K. Yu, Q. Gui, Y. Jiang, Z. Zhao, C. Shen, B. Wu and X. Chu, “Determination of 107 Pesticide Resi- dues in Vegetables Using Off-Line Dispersive Solid- phase Extraction and Gas Chroma-tography-tandem Mass Spectrometry,” Chinese Journal of Chromatography, Vol. 4, 2009, pp. 391-400.
P. Payá, M. Anastassiades, D. Mack, I. Sigalova, B. Tas- delen, J. Oliva and A. Barba, “Analysis of Pesticide Re- sidues Using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) Pesticide Multiresidue Method in Com- bination with Gas and Liquid Chromatography and Tan- dem Mass Spectrometric Detection,” Analytical and Bioanalytical Chemistry, Vol. 389, No. 6, 2007, pp. 1697- 1714. doi:10.1007/s00216-007-1610-7
C. Le-sueur, P. Knittl, M. Gartner, A. Mentler and M. Fuerhacker, “Analysis of 140 Pesticides from Conven- tional Farming Foodstuff Samples after Extraction with the Modified QuECh-eRS Method,” Food Control, Vol. 19, No. 9, 2008, pp. 906-914. doi:10.1016/j.foodcont.2007.09.002
T. D. Nguyen, J. E. Yu, D. M. Lee and G. H. Lee, “A Multiresidue Method for the Determination of 107 Pe- sticides in Cabbage and Radish Using QuEChERS Sam- ple Preparation Method and Gas Chromato-graphy Mass Spectrometry,” Food Chemistry, Vol. 110, No. 1, 2008, pp. 207-213. doi:10.1016/j.foodchem.2008.01.036
A. Garrido Frenich, J. L. Martínez Vidal, E. Pastor- Montoro and R. Romero-González, “High-Throughput Determination of Pesticide Residues in Food Commodi- ties by Use of Ultra-performance Liquid Chromatography —Tandem Mass Spectrometry,” Analytical and Bioanalytical Chemistry, Vol. 390, No. 3, 2008, pp. 947-959. doi:10.1007/s00216-007-1746-5
K. Ma?tovská, S. J. Le-hotay and M. Anastassiades, “Com- bination of Analyte Protec-tants to Overcome Matrix Ef- fects in Routine GC Analysis of Pesticide Residues in Food Matrixes,” Analytical Chemistry, Vol. 77, No. 24, 2005, pp. 8129-8137. doi:10.1021/ac0515576
A. Beyer and M. Biziuk, “Ap-plications of Sample Prepa- ration Techniques in the Analysis of Pesticides and PCBs in Food,” Food Chemistry, Vol. 108, 2008, pp. 669-680. doi:10.1016/j.foodchem.2007.11.024