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

Year 2018, , 133 - 141, 31.03.2018

Bahar Bayrak

https://doi.org/10.21597/jist.407860

Cited By: 2

Abstract

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.

Keywords

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

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

Abstract

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.

Keywords

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

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