Method Development and Validation for the Determination of Pesticide Residues in Water by GC-NPD

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; dedeksiyon ve miktar sınırı, doğrusallık ve doğruluk (tekrarlanabilirlik tekrarüretilebilirlik, geri kazanma) limitine göre değerlendirildi. Yöntem, on bir pestisit için 2.5-25 ?g L-1 aralığında ve metamidofos için 5-25 ?g L-1 aralığında doğrusaldır. Korelasyon katsayıları 0.992' ye eşit veya daha yüksektir. Dedeksiyon limitleri (LOD) 0.67 ve 2.23 ?g L-1arasındadır. Miktar sınırlamaları (LOQ) 2.24 ve 7.45 ?g L-1 arasında değişmektedir. 12 organofosforlu pestisit ve herbisit ile iki farklı konsantrasyon seviyesinde zenginleştirilmiş su numunelerinin geri kazanımı, yüksek konsantrasyonda %95'in üzerinde ve düşük konsantrasyonda %80' in üzerindedir. Tekrarlanabilirlik için, relatif standart sapma (RSD%) 2.79 ile 10.99 arasında ve tekrarüretilebilirlik için (RSD%), 1.56 ile %10.36 arasında değişmektedir. Geliştirilen yöntem, validasyon verilerine ve yüksek numune akışı ile uygun maliyetli oluşu gibi parametrelere göre su numunelerinde rutin uygulama için uygundur

Sudaki Pestisit Kalıntılarının Belirlenmesi için GC-NPD Kullanılarak Method Geliştirilmesi ve Validasyonu

A multi-residue method was developed for the determination of organophosphorous pesticides and Herbicide 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 pesticides and 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 pesticides and herbicide were over 95% in high concentration and 80% in low concentration. For repeatability, relative standard deviation (RSD%) ranged between 2.79 and 10.99%, and for reproducibility (RSD%) ranged between 1.56 and 10.36 %. The developed method is suitable for routine application in water samples in accordance with the validation data and the parameter as the high sample throughput and cost effective

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