Improvement of multi residue analysis method for pesticide residues in some fruits and vegetables using high pressure liquid chromatography (HPLC)

Yıl 2012, Cilt: 52 Sayı: 4, 375 - 394, 24.12.2012

Nuran Yigit , A. Öktem Gülderen Yentür

Öz

Yüksek Basınçlı Sıvı Kromatografisi (HPLC)-Diode Array Dedektör kullanılarak 19 tane pestisitin kalıntı analizine imkan sağlayan çoklu kalıntı analiz metodu geliştirilmiştir. Ekstraksiyon işleminde asetonitril, susuz magnezyum sülfat ve sodyum klorür ile temizleme işleminde susuz magnezyum sülfat ve primer sekonder amin kullanılmıştır. Metot geçerli kılma çalışmalarında pestisit içermeyen patlıcan, şeftali, domates, mandalina örnekleri kullanılmış ve sonuçlar kabul edilebilir aralıklarda bulunmuştur. Her bir pestisit için cihazın dedeksiyon limiti (IDL) ve Metot dedeksiyon limiti (EMDL) hesaplanmıştır. Matriksde hazırlanan kalibrasyon grafiklerinden elde edilen korelasyon katsayıları 0.99'dan yüksektir. Doğruluk için ortalama geri kazanımlar %75.39-121.95 arasında ve bağıl standart sapmalar (%RSD) %20'den düşüktür. Ayrıca kesinlik (gün içi tekrarlanabilirlik ve günler arası tekrar üretilebilirlik) için hesaplanan %RSD değerleri %10'dan düşük bulunmuştur. Geliştirilen metod basit, atığı az ve ekonomiktir. Kalıntı izleme programlarında kolaylıkla kullanılabileceği düşünülmektedir.

Anahtar Kelimeler

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Bazı meyve ve sebzelerde pestisit kalıntılarının analizinde yüksek basınçlı sıvı kromatografisi (HPLC) ile çoklu kalıntı analiz metodunun geliştirilmesi

Öz

Multi-residue analyse method using high-pressure liquid chromatography (HPLC) with Diode Array Detector was investigated for the determination of 19 pesticides. Acetonitrile, anhydrous magnesium sulphate and sodium chloride were used in extraction process via anhydrous magnesium sulphate and primary secondary amine were used in cleanup process. Pesticide free samples of eggplant, peach, tomato, mandarin were used for method validation studies and results were found at acceptable range. Instrument Detection Limit (IDL) and Estimated Method Detection Limit (EMDL) were calculated for each pesticide. Correlation coefficient which were acquired from matrix matched calibration graphs were higher than 0.99. Mean recoveries were between 75.39-121.95% and relative standart deviations (RSD%) were lower than 20% for accuracy. Also the RSD which were calculated for precision (intra-day repeatability and inter-day reproducibility) were found lower than 10%. It is thought that, this method can be used easily for residue monitoring programmes. It is simple, economic and has small waste.

Anahtar Kelimeler

Çoklu kalıntı analiz metodu, HPLC, pestisit kalıntısı, meyve, sebze

Kaynakça

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