Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu

Abstract

QuEChERS metodu ile “Golden Delicious” ve “Starking Delicious” elma çeşitlerinde chlorpyrifos etken maddenin kalıntı analizi için 0.05, 0.5 ve 5.0 mg/kg seviyelerinde zenginleştirme yapılarak validasyon gerçekleştirilmiştir. Analizler yapıldıktan sonra LC-MS/MS kullanılarak kromatografik ayrıştırma yapılmıştır. Matris etkisini elimine etmek için matrisli kalibrasyon (MC) kullanılmıştır. Bu yüzden, MCGolden D ve MCStarking D kalibrasyonları kullanılmıştır. Metodun validasyonu, gerçeğe yakınlık (accuracy), kalibrasyonun doğrusallığı, geri alım, cihaz dedeksiyon limiti, metodun tespit limiti, tekrar edilebilirlik ve kesinlik gibi kriterler ile gerçekleştirilmiştir. Her iki çözücü kalibrasyon kurvesi ve her iki matris kalibrasyon eğrisi 5-200 pg/µl aralığında lineer olarak bulunmuştur. Golden D örneğinden geri alımı; %8.36-14.03 tekrar edebilirlik değerleri ile %70.87-112.99 arasında bulunmuştur (ortalama geri alım %89.32). Starking D elma örneği için ise geri alım; %1.96-12.88 tekrar edebilirlik değerleri ile  %69.08-100.3 arasında bulunmuştur (ortalama geri alım %79.82). Tüm metodun geri alımı %15.68 relatif standart sapma ile  %84.60 olarak bulunmuştur. Tüm bulgular olması gereken geri alım sınırlarına (%70-120) ve tekrar edebilirlik kabul oranı için belirtilen değerlere (RSD ≤% 20) uygundur.

Keywords

• matris etkisi,metot geçerliliği,pestisit kalıntısı,QuEChERS

Method Validation for the Chlorpyrifos in Apples by QuEChERS Analysis Method

Abstract

QuEChERS method was validated using “Golden Delicious ’’ and “Starking Delicious” apples, fortified with 0.05, 0.5 and 5.0 µg/g chlorpyrifos. Analyses were performed by QuEChERS method then chromatographic separation was performed by using LC-MS/MS. Calibration with matrix (MC) was used to compensate matrix effect. Thus MCGolden D and MCStarking D were used for quantification. The method validated by using following parameters; accuracy, linearity of calibration, recovery, instrument detection limit, estimated method detection limit, repeatability and precision. Calibration curve of solvent and both matrix matched calibration curve were the linear over the range of 5–200 pg/µl. Recovery of chlorpyrifos from Golden D apples were between 70.87–112.99% (mean recovery 89.32%) with the repeatability of 8.36-14.03%. Similarly recovered chlorpyrifos from Starking D apples ranged between 69.08–100.3% (mean recovery 79.82%) with the repeatability of 1.96-12.88%. For overall recovery of the procedure was 84.60% ( RSD= 15.68%). These all figures comply with the determined values for average recovery limits (70-120%) and precision (RSD ≤ 20%).

Keywords

• matrix effect,method validation,pesticide residue,QuEChERS

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