Çevresel Su Örneklerinde GC/MSD ile Pestisit Analizi ve Metot Validasyonu

Yıl 2017, , 407 - 414, 27.12.2017

Şeyda Kıvrak Tolga Göktürk

https://doi.org/10.17100/nevbiltek.321723

Cited By: 4

Öz

Bu
çalışmada, su numunelerinde 130'dan fazla pestisit kalıntısının ppb (μg/L)
düzeyinde belirlenmesinde kullanılabilecek hızlı ve çoklu bir analiz yöntemi
önerilmiştir. Bu amaçla, analit konsantrasyonunun zenginleştirilmesi için bir
Kuderna-Danish Evaporatif Konsantratör ve SIM (Selective Ion Monitoring)
modunda çalışan gaz kromotografisi (GC) ile birleştirilmiş kütle spektrometresinin
(MSD) kullanıldığı bir yöntem geliştirildi ve çoklu pestisit analizi için
validasyonu yapıldı. Kromatografik analizde, pestisitlerin düşük
konsantrasyonlarda dahi yüksek hassasiyetle tespit edilebilmesi gerektiğinden
dolayı 30m HP-5 MS UI kapiler GC kolonu kullanıldı. Geliştirilen yöntemle miktar tayin limitleri 1.8
ve 29.2 ng.L^-1 olarak belirlendi. Yöntem, bileşiklerin çoğunda
sırasıyla 10 ppb ve 50 ppb seviyeleri için 70.1-116.5 % ve 70.7 – 114.0% aralıklarında
ortalama geri kazanım sağladı. Pestisitlerin birbirinden çok farklı kimyasal
yapıları, analizi yapılan tüm bileşikler için iyi bir geri kazanım sağlamayı
zorlaştırmış olmasına rağmen sonuçların hassasiyetinin mükemmel olduğu
değerlendirilebilir. Metodun seçiciliği, hesaplama ve tanımlama iyonlarının
bağıl oranı yoluyla değerlendirildi ve değerlendirme sonucunda yeterli kabul
edildi. Gerçek numunelerdeki analizler, enstrümantal yeterlilik kriterlerini ve
sistem uygunluğu değerlendirmesini karşılamıştır. Böylelikle, 130 pestisitin
nitel ve nicel tayinleri yapılmıştır.

Anahtar Kelimeler

Pestisit, Su, Aldrin, Validasyon, GC/MSD

Pesticide Analysis and Method Validation with GC/MSD Instrument in Environmental Water Samples

Öz

In
this study, a rapid and multiple method has been proposed which can be used in
determination of more than 130 pesticide residues at ppb (μg/L) level in water
samples. For this purpose, a Kuderna-Danish Evaporative Concentrator, which was
used for enrichment of the analyte concentration in the samples and gas
chromatography coupled mass spectrometry in the selective ion monitoring (SIM)
mode was developed and validated for the multi-class determination of
pesticides. In the analysis, a 30m HP-5 MS UI capillary GC columns was used. The
high sensitivity of chromatographic analysis was necessary, due to that these
pesticides must be determined at low concentrations. The method presented
quantification limits between 1.8 and 29.2 ng.L^-1. Most of the
compounds presented mean recoveries between 70.1-116.5 % and 70.7 – 114.0% at
10 ppb and 50 ppb levels, respectively. Although the difference in chemical
natures of the pesticides made difficult to attain good recovery for all of the
compounds evaluated, the precision of the results was excellent. The
selectivity of the method was evaluated through the relative intensity of
quantification and qualification ions and was considered adequate. Analysis in
real samples met criteria for instrumental qualification and the system
suitability evaluation. Thus, qualitative and quantitative determinations of
130 pesticide were done.

Anahtar Kelimeler

Pesticide, Water, Aldrin, Validation, GC/MSD

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