Yaş Üzümde Pestisit Kalıntılarının GC [Çoklu-Dedektörlere(µ-ECD, MSD, Dual-FPD) sahip gaz kromatografisi] ile Çoklu Kalıntı Tayini için Analiz Yönteminin Geliştirilmesi

Yıl 2018, Cilt: 20 Sayı: 60, 876 - 889, 15.09.2018

Gözde Türköz Bakırcı Yaşar Hışıl

Öz

Ülkemizde yaş üzümdeki pestisit kalıntılarının tayini
için hızlı, ucuz, kolay, güvenli, etkili, kesin sonuç veren  ekstraksiyon
ve analiz yöntemi geliştirilmiştir. Geliştirilen metotta, örnekler basınç
altında sıvı TFE çözgeni kullanılarak ekstrakte edilmektedir. Elde edilen
ekstraktlar GC [Çoklu-Dedektörlere(µ-ECD, MSD, Dual-FPD) sahip gaz
kromatografisi] ile analiz edilmektedir. Bu metot, isomerleri ile birlikte 61
aktif maddenin GC [Çoklu-Dedektörlere(µ-ECD, MSD, Dual-FPD) sahip gaz
kromatografisi]’de doğrulama ve kantitatif analizine imkan vermektedir. Metot,
geçerli kılınmış (valide edilmiş) ve sonuçlar kabul edilir aralıklarda
bulunmuştur. Pestisitlerin gözlenebilme sınırı (LOD) ve tayin sınırı (LOQ),
Maksimum Kalıntı Limitleri (MRL)’nden düşük, matrikste hazırlanan
kalibrasyonlardan elde edilen korelasyon katsayıları (R2) 0.99’dan yüksek, geri
kazanımlar % 70-120 arasında ve relatif standart sapmaları (% RSD, doğruluk ve
tekrarlanabilirlik) %20’den düşük bulunmuştur.

Anahtar Kelimeler

Üzüm, GC/ECD/FPD/MSD, Pestisit, Çoklu kalıntı analizi

Development of Multi Residue Analysis Method in Determining Pesticide Residues on Grapes Simultaneously by GC [Gas Chromatography Having Multi-Detector (µ-ECD, MSD, Dual-FPD)]

Öz

Determination of pesticide residues in fruits and vegetables for giving
fast, cheap, easy, safe, effective, rugged results of the extraction and
analysis methods have been developed. In developed method, the samples were
extracted using pressurized fluid solvent (1,1,1,2-TFE) and extracts were
analysed by GC [having multi-detector 
(μ-ECD, MSD, Dual-FPD)] with gas chromatography]. This method gives the
chance for verifing and quantitation for together isomers of 61 active
substance by using GC. Method was validated and the results were accepted in
normal ranges. Limit of detection (LOD) and quantitation (LOQ) values of active
substances were found lower than Maximum Residue Limits (MRL) and  correlation coefficients (R2) were higher
than 0.99 with matrix matched calibration and recoveries were found between
70-120 % and relative standart deviations were lower than  20 % (RSD %, for accuracy and repeatability).

Anahtar Kelimeler

Grapes, GC/ECD/FPD/MSD, Pesticides, Multi residue analysis

Kaynakça

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