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

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)]

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).

Keywords:

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

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