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

Abstract

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.

Keywords

• Pestisit,Su,Aldrin,Validasyon,GC/MSD

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

Abstract

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.

Keywords

• Pesticide,Water,Aldrin,Validation,GC/MSD

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