OYA AYDIN URUCU, Ece Kök YETİMOĞLU, Deniz DEVECİOĞLU

Determination of Chlorpyrifos Residues in Cherry Samples by Headspace Solid Phase Microextraction Coupled with Gas Chromatography Mass Spectrometry

A method based on a direct immersion solid phase microextraction gas chromatography – mass spectrometry (DI-SPME-GC-MS) was developed for the quantitative determination of chlorpyrifos (CRF) residues in cherry samples. The performance of three kinds of commercial fiber coatings: PA (polyacrylate, 85µm), PDMS–DVB (polydimethylsiloxane–divinylbenzene 65 mm) and PDMS (polydimethylsiloxane, 100 mm) were compared. Various parameters affecting SPME procedures such as temperature, extraction and desorption times, salinity, stirring rate were investigated. The analytes from all sample extracts were preconcentrated for 30 minutes in the SPME fiber at 60 °C and then the fiber was desorbed by heating at 250 °C for 10 minutes in the gas chromatography injection port. Limits of detection (LOD) and quantitation (LOQ) values were 0.03 µg/L and 0.1 µg/L, respectively. An average recovery range was 93-98% with relative standard deviation (RSD) < 10 %.

Direkt Daldırma Katı Faz Mikroekstraksiyon Yöntemi İle Kiraz Örneklerinde Klorpirifos Kalıntılarının Gaz Kromatografisi Kütle Spektrometresinde Tayini

Direkt daldırma katı fazlı mikroekstraksiyon ile kiraz örneklerinde klorpirifos kalıntılarının gaz kromatografisinde tayini (DI-SPMEGC-MS) için bir yöntem geliştirilmiştir. Üç çeşit ticari fiber kaplamanın, PA (poliakrilat, 85 um), PDMS-DVB (polidimetilsiloksan-divinilbenzen 65 mm) ve PDMS (polidimetilsiloksan, 100 mm), performansı karşılaştırıldı. Katı Fazlı Mikroekstraksiyon prosedürlerini etkileyen sıcaklık, ekstraksiyon ve desorpsiyon süreleri, tuzluluk, karıştırma oranı gibi çeşitli parametreler incelendi. Tüm numune ekstraktlarından alınan analitler, 30 dakika boyunca 60 ° C’ de SPME fiberine adsorbe edilmiş ve daha sonra fiber, gaz kromatografi enjeksiyon portunda 10 dakika boyunca 250 ° C’de ısıtılarak desorpsiyon sağlanmıştır. Yöntemin tespit sınırı (LOD) ve tayin sınırı (LOQ) değerleri sırasıyla 0,03 µg / L ve 0,1 µg / L dir. Yöntemin ortalama geri kazanım aralığı % 93-98 iken bağıl standart sapma (RSD)

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