Development of a Multiresidue Methods for The Simultaneous Determination of Pesticide Residues in Water by GC/Mass Spectrometry

Abstract

A Multi-residue methods were developed for the determination of pesticides by liquid-liquid extraction (LLE) and followed by gas chromatographymass spectrometry (GC/Mass).
The method was evaluated with respect to the limit of detection and quantification, linearity and accuracy. For GC/MS, LODs were between 1.27 µg/L and 4.24 µg/L and LOQs were between 4.23 µg/L and 14.15 µg/L. Recoveries were obtained over 96% in high concentration and 92% in low concentration. Repeatabilities were varied from 3.81 to 14.40 (except for simazine) and reproducibilities (RSD%) were varied from 5.81 to17.32.

Keywords

• Pesticides
• Method validation
• GC/MS

Gaz Kromatografisi/Kütle Spektrometrisi ile Sudaki Pestisit Kalıntılarının Eşzamanlı Olarak Belirlenmesi için Çoklu Kalıntı Metodu Geliştirilmesi

Abstract

Sıvı-sıvı ekstraksiyonu (LLE) ve ardından gaz kromatografisi kütle spektrometrisi (GC/MS) ile pestisitlerin tayini için çoklu kalıntı yöntemi geliştirildi. Yöntem; her bir pestisit için nicel tayin sınırı (LOQ) ve belirtme alt sınırı (LOD), doğrusallık ve doğruluk parametrelerine göre değerlendirildi. GC/MS için, LOD değerleri 1.27 μg/L ile 4.24 μg/L arasında ve LOQ değerleri 4.23 μg/L ile 14.15 μg/L arasında elde edildi. Geri kazanımlar, yüksek konsantrasyonda % 96 ve düşük konsantrasyonda % 92 olarak bulundu. Tekrarlanabilirlik (simazin hariç) 3.81 ila 14.40 arasında değişirken, yeniden üretilebilirlik (RSD%) 5.81 ila 17.32 arasında değişmiştir.

Keywords

• Pestisitler
• Metot validasyonu
• GC/MS

References

1. Beltran, J., Lopez, F. J., Cepria, O.,Hernandez, F. 1998. Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples. Journal of Chromatography A, 808(1-2), 257-263.
2. Castilho, J. A. A., Fenzl, N., Guillen, S. M.,Nascimento, F. S. 2000. Organochlorine and organophosphorus pesticide residues in the Atoya river basin, Chinandega, Nicaragua. Environmental Pollution, 110(3), 523-533.
3. Commission, E. (2013). Method validation and quality control procedures for pesticides residues analysis in food and feed. (Type No. Report Number).Costa, L. L., Sant ana, E. S., Suchara, E. A., Benato, V. S.,Carasek, E. 2008. Determinação de herbicidas usados no cultivo de arroz irrigado na região sul do estado de Santa Catarina através da SPME-GC-ECD. Química Nova, 31(1), 79.
4. de Souza Pinheiro, A.,de Andrade, J. B. 2009. Development, validation and application of a SDME/GC-FID methodology for the multiresidue determination of organophosphate and pyrethroid pesticides in water. Talanta, 79(5), 1354-1359.
5. Domotorova, M.,Matisova, E. 2008. Fast gas chromatography for pesticide residues analysis. Journal of Chromatography A, 1207(1-2), 1-16.Dorea, H. S., Tadeo, J. L.,SanchezBrunete, C. 1996. Determination of organophosphorus pesticide residues in fruits by gas chromotography with ITD and NPD detection. Chromatographia, 43(7-8), 380-386.
6. Driss, M., Hennion, M.-C.,Bouguerraca, M. 1993. Determination of carbaryl and some organophosphorus pesticides in drinking water using on-line liquid chromatographic preconcentration techniques. Journal of Chromatography A, 639(2), 352-358.Jin, B. H., Xie, L. Q., Guo, Y. F.,Pang, G. F. 2012. Multi-residue detection of pesticides in juice and fruit wine: A review of extraction and detection methods. Food Research International, 46(1), 399-409.
7. Komatsu, E.,Vaz, J. M. 2004. Otimização dos parâmetros de extração para determinação multiresíduo de pesticidas em amostras de água empregando microextração em fase sólida. Química Nova, 27(5), 720-724.
8. Menezes Filho, A., dos Santos, F. N.,Pereira, P. A. d. P. 2010. Development, validation and application of a method based on DI-SPME and GC–MS for determination of pesticides of different chemical groups in surface and groundwater samples. Microchemical Journal, 96(1), 139-145.

9. Park, J. H., Iqbal Rouf Mamun, M., Abd El‐Aty, A., Na, T. W., Choi, J. H., Ghafar, M., Kim, K. S., Kim, S. D.,Shim, J. H. 2011. Development and validation of a multiresidue method for determination of 37 pesticides in soil using GC‐NPD. Biomedical Chromatography, 25(9), 1003-1009.Piedra, L., Tejedor, A., Hernando, M. D., Aguera, A., Barcelo, D.,Fernandez-Alba, A. 2000. Screening of antifouling pesticides in sea water samples at low ppt levels by GC-MS and LC-MS. Chromatographia, 52(9-10), 631-638.
10. Rocha, M. J., Ribeiro, M. F., Cruzeiro, C., Figueiredo, F.,Rocha, E. 2012. Development and validation of a GC-MS method for determination of 39 common pesticides in estuarine water–targeting hazardous amounts in the Douro River estuary. International Journal of Environmental Analytical Chemistry, 92(14), 1587-1608.Suman, P.,Singh, D. K. 2011. Estimating the uncertainty of pesticide residue analysis from mango using multi-residue analysis and validation of method. Toxicological and Environmental Chemistry, 93(10), 1880-1896.
11. Vidal, J. L. M., Liebanas, F. J. A., Rodriguez, M. J. G., Frenich, A. G.,Moreno, J. L. F. 2006. Validation of a gas chromatography/triple quadrupole mass spectrometry based method for the quantification of pesticides in food commodities. Rapid Communications in Mass Spectrometry, 20(3), 365-375.