Rapid Residue Analysis of Sulfonylurea Herbicides in Surface Water: Methodology and Residue Findings in eastern Tiaoxi River of China

Ninghui  Song; Min  Guo; Lili  Shi

doi:10.4236/msce.2016.46006

Ninghui Song, Min Guo, Lili Shi

Abstract:

A new method combining QuEChERS (quick, easy, cheap, effective, rugged and safe) and DLLME (dispersive liquid–liquid microextraction) for the simultaneous determination of residues of ten sulfonylurea herbicide in water using UPLC-MS/MS was developed and validated. Analytes were extracted and purified with QuEChERS and concentrated in chlorobenzene by applying the DLLME procedure. Several extraction parameters were tested, such as volume, extractive solvent by the QuEChERS method and subsequently used for DLLME, selection of extractive solvent and its volume, was tested. The developed method was validated on the basis of international guidelines. Mean recoveries ranged from 81.2 to 104.9%. Repeatability and reproducibility were lower than 10%. Limits of detection (LODs) and quantification (LOQs) were below 0.074 μg/L and 0.244 μg/L, respectively. Decision limit (CCα) and detection capability (CCβ) were calculated and CCβ ranged from 0.101 μg/L (pyrazosulfuron-ethyl) to 0.260 μg/L (nicosulfuron). Finally, when the method was applied to real samples, traces of three compounds were found in 42 samples and only thifensulfuon-methyl was detected above the LOQ in three samples at 0.17-0.20 μg/L.

Keywords: Sulfonylurea herbicides, pesticide residues, UPLC-MS/MS, QuEChERS, DLLME

Cite this paper: Song, N. , Guo, M. and Shi, L. (2016) Rapid Residue Analysis of Sulfonylurea Herbicides in Surface Water: Methodology and Residue Findings in eastern Tiaoxi River of China. Journal of Materials Science and Chemical Engineering, 4, 41-50. doi: 10.4236/msce.2016.46006.

References

[1] Gure, A., Lara, F.J., Moreno-González, D., Megersa, N., del Olmo-Iruela, M. and García-Campa?a, A.M. (2014) Salting-Out Assisted Liquid-Liquid Extraction Combined with Capillary HPLC for the Determination of Sulfonylurea Herbicides in Environmental Water and Banana Juice Samples. Talanta, 127, 51-58. http://dx.doi.org/10.1016/j.talanta.2014.03.070

[2] Yan, C., Zhang, B., Liu, W., Feng, F., Zhao, Y. and Du, H. (2011) Rapid De-termination of Sixteen Sulfonylurea Herbicides in Surface Water by Solid Phase Extraction Cleanup and Ultra-High-Pressure Liquid Chromatography Coupled with Tandem Mass Spectrometry. J Chromatogr B, 879, 3484-3489.http://dx.doi.org/10.1016/j.jchromb.2011.09.028

[3] Jenny, K. andStina, A. (2008) Monitoring of Sulfonylurea Herbi-cides in Stream Water Draining Intensively Cultivated Areas in Southern Sweden during a 9-Year Period(1998-2006). http://pub.epsilon.slu.se/5401/1/kreuger_j_et_al_101101.pdf

[4] De Lafontaine, Y., Beauvais, C., Cessna, A.J., Gagnon, P., Hudon, C. and Poissant, L. (2014) Sulfonylurea Herbicides in an Agricultural Catchment Basin and Its Adjacent Wetland in the St. Lawrence River Basin. Sci Total Environ, 479-480, 1-10.http://dx.doi.org/10.1016/j.scitotenv.2014.01.094

[5] Zhou, Q.X., Liu, J.F., Cai, Y.Q., Liu, G.G. and Jiang, G.B. (2003) Micro-Porous Membrane Liquid-Liquid Extraction as an Enrichment Step Prior to Nonaqueous Capillary Electrophoresis Determination of Sulfonylurea Herbicides. Microchem J, 74, 157-163.http://dx.doi.org/10.1016/S0026-265X(03)00003-1

[6] Ayano, E., Kanazawa, H., Ando, M. and Nishimura, T. (2004) Determination and Quantitation of Sulfonylurea and Urea Herbicides in Water Samples Using Liquid Chromatography with Elec-trospray Ionization Mass Spectrometric Detection. Anal ChimActa, 507, 211-218.http://dx.doi.org/10.1016/j.aca.2003.11.027

[7] Losito, I., Amorisco, A., Carbonara, T., Lofiego, S.andPalmisano, F. (2006) Simultaneous Determination of Phenyl- and Sulfonyl-Urea Herbicides in River Water at Sub-Parts-per-Billion Level by On-Line Preconcentration and Liquid Chromatography-Tandem Mass Spectrometry. Anal ChimActa, 575, 89-96. http://dx.doi.org/10.1016/j.aca.2006.05.063

[8] Degelmann, P., Egger, S., Jürling, H., Müller, J., Niessner, R. and Knopp, D. (2006) Determination of Sulfonylurea Herbicides in Water and Food Samples Using Sol-Gel Glass-Based Immunoaffinity Extraction and Liquid Chromatography-Ultraviolet/Diode Array Detection or Liquid Chromatography-Tandem Mass Spectrometry. Food Chem, 54, 2003-2011.http://dx.doi.org/10.1021/jf052718+

[9] Liu, J.F., Chao, J.B., Jiang, G.B., Cai, Y.Q. and Liu, J.M. (2003) Trace Analysis of Sulfonylurea Herbicides in Water by On-Line Continuous Flow Liquid Membrane Extraction-C18 Precolumn Liquid Chromatography with Ultraviolet Absorbance Detection. J Chromatogr A, 995, 21-28.http://dx.doi.org/10.1016/S0021-9673(03)00515-6

[10] [10] Penmetsa, K.V., Leidy, R.B. and Shea, D. (1997) Enantiomeric and Isomeric Separation of Herbicides Using Cyclodextrin-Modified Capillary Zone Electrophoresis. J Chromatography A, 790, 225-234. http://dx.doi.org/10.1016/S0021-9673(97)00765-6

[11] Anastassiades, M., Lehotay, S.J., ?tajnbaher, D. and Schenck, F.J. (2003) Fast and Easy Multiresidue Method Employing Acetonitrile Extraction/Partitioning and “Dispersive Solid-Phase Extraction” for the Determination of Pesticide Residues in Produce. J AOAC Int, 86, 412-431.

[12] Mastovska, K. andLehotay, S.J. (2006) Rapid Sample Preparation Method for LC-MS/MS or GC-MS Analysis of Acrylamide in Various Food Matrices. J Agr Food Chem, 54, 7001-7008.http://dx.doi.org/10.1021/jf061330r

[13] Seccia, S., Albrizio, S., Fidente, P. and Montesano, D. (2011) Development and Validation of a Solid-Phase Extraction Method Coupled to High-Performance Liquid Chromatography with Ultraviolet-Diode Array Detection for the Determination of Sulfonylurea Herbicide Residues in Bovine Milk Samples. J Chromatogr A, 1218, 1253-1259. http://dx.doi.org/10.1016/j.chroma.2011.01.006

[14] Zhao, P., Wang, L., Zhou, L., Zhang, F., Kang, S. and Pan, C. (2012) Multi-Walled Carbon Nanotubes as Alternative Reversed-Dispersive Solid Phase Extraction Materials in Pesticide Multi-Residue Analysis with QuEChERS Method. J Chromatogr A,1225, 17-25.http://dx.doi.org/10.1016/j.chroma.2011.12.070

[15] Lehotay, S.J., Son, K., Kwon, H., Koesukwiwat, U., Fu, W., Mastovska, K. andLeepipatpiboon, N. (2010) Comparison of QuEChERS Sample Preparation Methods for the Analysis of Pesticide Residues in Fruits and Vegetables. J Chromatogr A, 1217, 2548-2560.http://dx.doi.org/10.1016/j.chroma.2010.01.044

[16] Cunha, S.C. and Fernandes, J.O. (2011) Multipesticide Residue Analysis in Maize Combining Acetonitrile-Based Extraction with Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry. J Chromatogr A, 1218, 7748-7757.http://dx.doi.org/10.1016/j.chroma.2011.08.066

[17] Rezaee, M., Assadi, Y., Hosseini, M.R.M., Aghaee, E., Ahmadi, F. andBerijani, S. (2006) Determination of Organic Compounds in Water Using Dispersive Liquid-Liquid Microextraction. J Chromatogr A, 1116, 1-9. http://dx.doi.org/10.1016/j.chroma.2006.03.007

[18] Wu, Q., Wang, C., Liu, Z., Wu, C., Zeng, X., Wen, J. and Wang, Z. (2009) Dispersive Solid-Phase Extraction Followed by Dispersive Liquid-Liquid Microextraction for the Determination of Some Sulfonylurea Herbicides in Soil by High-Performance Liquid Chromatography. J Chromatogr A, 1216, 5504-5510. http://dx.doi.org/10.1016/j.chroma.2009.05.062

[19] Caldas, S.S., Costa, F.P. and Primel, E.G. (2010) Validation of Method for Determination of Different Classes of Pesticides in Aqueous Samples by Dispersive Liquid-Liquid Microextraction with Liquid Chromatography-Tandem Mass Spectrometric Detection. Anal ChimActa, 665, 55-62.http://dx.doi.org/10.1016/j.aca.2010.03.004

[20] Sui, K., Li, J., Wei, F., Chu, X., Zhao, S. and Wang, Y. (2006) Simultaneous Determination of Twelve Sulfonyl Urea Herbicide Residues in Rice by High Performance Liquid Chromatography with Solid-Phase Extraction. Chin J Chromatogr, 24, 152-156.