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

Öz

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.

Anahtar Kelimeler

• Environmental pollution,GC/NPD,method validation,multi-residue analysis,pesticide

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

Öz

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 μg L-1 aralığında ve metamidofos için 5-25 μg L-1 aralığında

doğrusaldır. Korelasyon katsayıları 0.992’ ye eşit veya daha yüksektir. Dedeksiyon limitleri (LOD) 0.67 ve 2.23 μg L-1

arasındadır. Miktar sınırlamaları (LOQ) 2.24 ve 7.45 μg 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.

Anahtar Kelimeler

• Çevre kirliliği,çoklu kalıntı analizleri,GC/NPD,metod validasyonu,pestisit

Kaynakça

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