TY  - JOUR
T1  - Sudaki Pestisit Kalıntılarının Belirlenmesi için GC-NPD Kullanılarak Method Geliştirilmesi ve Validasyonu
TT  - Method Development and Validation for the Determination of Pesticide Residues in Water by GC-NPD
AU  - Bayrak, Bahar
PY  - 2018
DA  - March
Y2  - 2017
DO  - 10.21597/jist.407860
JF  - Journal of the Institute of Science and Technology
JO  - J. Inst. Sci. and Tech.
PB  - Igdir University
WT  - DergiPark
SN  - 2536-4618
SP  - 133
EP  - 141
VL  - 8
IS  - 1
LA  - tr
AB  - Organik fosforlu pestisitlerin ve herbisitlerin sıvı-sıvı ekstraksiyonu (LLE) ve ardından gaz kromatografisiazot-fosfor dedektörü (GC / NPD) ile belirlenmesi için bir çoklu kalıntı yöntemi geliştirildi. Metod; dedeksiyonve miktar sınırı, doğrusallık ve doğruluk (tekrarlanabilirlik tekrarüretilebilirlik, geri kazanma) limitine göredeğerlendirildi. Yöntem, on bir pestisit için 2.5-25 μg L-1 aralığında ve metamidofos için 5-25 μg L-1 aralığındadoğrusaldır. Korelasyon katsayıları 0.992’ ye eşit veya daha yüksektir. Dedeksiyon limitleri (LOD) 0.67 ve 2.23 μg L-1arasındadır. Miktar sınırlamaları (LOQ) 2.24 ve 7.45 μg L-1 arasında değişmektedir. 12 organofosforlu pestisitve herbisit ile iki farklı konsantrasyon seviyesinde zenginleştirilmiş su numunelerinin geri kazanımı, yüksekkonsantrasyonda %95’in üzerinde ve düşük konsantrasyonda %80’ in üzerindedir. Tekrarlanabilirlik için, relatifstandart sapma (RSD%) 2.79 ile 10.99 arasında ve tekrarüretilebilirlik için (RSD%), 1.56 ile %10.36 arasındadeğişmektedir. Geliştirilen yöntem, validasyon verilerine ve yüksek numune akışı ile uygun maliyetli oluşu gibiparametrelere göre su numunelerinde rutin uygulama için uygundur.
KW  - Çevre kirliliği
KW  - çoklu kalıntı analizleri
KW  - GC/NPD
KW  - metod validasyonu
KW  - pestisit
N2  - A multi-residue method was developed for the determination of organophosphorous pesticides andHerbicide by liquid-liquid extraction (LLE) and followed by gas chromatography-nitrogen-phosphorus detector(GC/NPD). The method was evaluated with respect to the limit of detection and quantification, linearity and accuracy(repeatability, reproducibility, recovery). The method is linear over the range 2.5 -25 μg L-1 for eleven pesticidesand 5-25 μg L-1 for methamidophos. Correlation coefficients were higher or equal to 0.992. The limits of detection(LODs) were between 0.67 and 2.23 μg L-1. The limits of quantification (LOQs) ranged from 2.24 and 7.45 μg L-1.Recoveries of fortified water samples in two different concentration levels with 12 organophosphorous pesticidesand herbicide were over 95% in high concentration and 80% in low concentration. For repeatability, relative standarddeviation (RSD%) ranged between 2.79 and 10.99%, and for reproducibility (RSD%) ranged between 1.56and 10.36 %. The developed method is suitable for routine application in water samples in accordance with thevalidation data and the parameter as the high sample throughput and cost effective.
CR  - Beltran, J., Lopez, F., Cepria, O., Hernandez, F., 1998. Solid-phase microextraction for quantitative analysis of organophosphorus pesticides in environmental water samples. Journal of Chromatography A 808, 257-263.
CR  - Bempelou, E.D., Liapis, K.S., 2006. Validation of a multi-residue method for the determination of pesticide residues in apples by gas chromatography. International Journal of Environmental Analytical Chemistry 86, 63-68.
CR  - Cabrera, L.d.C., Costa, F.P., Primel, E.G., 2008. Estimativa de risco de contaminação das águas por pesticidas na região sul do estado do RS.
CR  - Canbay, H., Öğüt, S., Yılmazer, M., 2014. Pesticide residues analysis in lake water and sediment samples from the Golcuk National Park. Water resources 41, 97-104.
CR  - Castilho, J., Fenzl, N., Guillen, S.M., Nascimento, F., 2000. Organochlorine and organophosphorus pesticide residues in the Atoya river basin, Chinandega, Nicaragua. Environmental Pollution 110, 523-533.
CR  - 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, 79.
CR  - Dorea, H., Tadeo, J., Sanchez-Brunete, C., 1996. Determination of organophosphorus pesticide residues in fruits by gas chromatography with ITD and NPD detection. Chromatographia 43, 380-386.
CR  - Dömötörová, M., Matisová, E., 2008. Fast gas chromatography for pesticide residues analysis. Journal of Chromatography A 1207, 1-16.
CR  - 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, 352-358.
CR  - Environmental Protection Agency (EPA), 1990. National survey of pesticides in drinking water wells. Phase I Report. Office of Water and Office of Pesticides Programs, U.S. Government Printing Office Washington, DC.
CR  - Jin, B., Xie, L., Guo, Y., Pang, G., 2012. Multi-residue detection of pesticides in juice and fruit wine: a review of extraction and detection methods. Food research international 46, 399-409.
CR  - 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, 720-724.
CR  - 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, 139-145.
CR  - 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, 1003-1009.
CR  - 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, 1587-1608.
CR  - SANCO, 2004. Quality control procedures for pesticide residue analysis. Document N8. SANCO/10476/2003. European Commission, Directorate General Health and Consumer Protection.
CR  - Suman, P., Singh, D.K., 2011. Estimating the uncertainty of pesticide residue analysis from mango using multi-residue analysis and validation of method. Toxicological & Environmental Chemistry 93, 1880-1896.
CR  - Tian, F., Liu, W., Fang, H., An, M., Duan, S., 2014. Determination of six organophosphorus pesticides in water by single-drop microextraction coupled with GC-NPD. Chromatographia 77, 487-492.
CR  - Vidal, J., Liébanas, F., Rodríguez, M., Frenich, A.G., Moreno, J., 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, 365-375.
UR  - https://doi.org/10.21597/jist.407860
L1  - https://dergipark.org.tr/en/download/article-file/444051
ER  -