Determination of organochlorinated pesticide residues by gas chromatography - mass spectrometry after elution in a florisil column

Bu çalışmanın amacı, rutin analizler için gaz kromatografi-kütle spektrometre (GC-MS) ile α-hekzaklorosiklohekzan (α-HCH), hekzaklorobenzen (HCB), heptaklor (HC), aldrin (ALD), 4,4-diklorodifenildikloroetilen (4,4-DDE) and 4,4-diklorodifeniltrikloroetan (4,4-DDT) kalıntılarının belirlenmesi için kolay bir analitik yöntem geliştirmektir. Örnek olarak tavuk kaslarından yararlanıldı. Örnek hazırlama aşamasında, florisil dolgu kolonu kullanıldı ve iyi bir performans elde edildi. Ortalama kesinlik ve doğruluk aralığı sırasıyla %8.03-24.00 ve %-4.36-30.67, (n=6). Ortalama geri kazanım farklı düzeydeki eklenmiş doku örnekleri için (25, 50, 100 ng/g) %95.74 ve %130.67 arasındadır. Ortalama gün içi ve arası kesinlik

Anahtar Kelimeler:

DDE, GC-MS, HCH, aldrin, analitik yöntemler, heptaklor, hekzaklorobenzen, kütle spektrometrisi, organoklorlu zararlı öldürücüler, zararlı öldürücü kalıntıları

Organik klorlu pestisid kalıntılarının florisil kolonda ayrılmasından sonra gaz kromatografi - kütle spektrometre ile belirlenmesi

The purpose of the present study was to develop an easy analytical method for determining α-hexachlorocyclohexane(α-HCH), hexachlorobenzene (HCB), heptachlor (HC), aldrin (ALD), 4,4-dichlorodiphenyldichloroethylene (4,4-DDE) and 4,4dichlorodiphenyltrichloroethane (4,4-DDT) residues by gas chromatography with mass spectrometre (GC–MS) for routineanalysis. Chicken muscles were utilized as samples in this study. A florisil packed column was used in sample preparation stepand showed good performance. The average precision and accuracy ranged 8.03-24.00% and -4.36-30.67%, respectively (n=6).The average recoveries were between 95.74 and 130.67% for various spiking levels (25, 50, 100 ng/g). The average of inter- andintra-day precision was <13 and the limits of detection were ranged 7-19 ng/g, depending on different organochlorinated (OC)pesticides. In conclusion, the extraction method used in the present study was inexpensive (do not require skilled operators,high volume of solvent or costly apparatus), easy and rapid. Additionally, the validation parameters show that the proposedmethod in this study is sensitive, reproducible and reliable alternative to the normally used methods. Thus, it could efficientlybe used in the routine and monitoring studies so that several samples can be run in parallel.

Keywords:

DDE, GC-MS, HCH, aldrin, analytical methods, heptachlor, hexachlorobenzene, mass spectrometry, organochlorine pesticides, pesticide residues,

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