Elmalarda İmidacloprid ve Dimethoate Kalıntıları için QuEChERS ve LC- MS/MS ile Metot Validasyonu

Pestisit kalıntı analizlerinde kullanılan tüm metotların, orijinal laboratuvar örneklerinin analizinden önce validasyonu yapılmalıdır. Bu çalışmada elmalarda imidacloprid ve dimethoate kalıntı analizi için analiz prosedürünün valide edilmesi amaçlanmıştır. Bu amaçla hiçbir ilaçlama yapılmamış Golden Delicious ve Starking Delicious elma örnekleri homojenize edilmiş ve pestisitlerle 3 farklı seviyede zenginleştirilmiştir. 10 g elma örneği QuEChERS yöntemi ile ekstraksiyon ve clean up işlemine tabi tutulmuştur. Takiben LC-MS/MS sisteminde imidacloprid ve dimethoate analizleri yapılmıştır. Her iki pestisit ve elma çeşiti için matris etkisi önemli bulunduğundan, miktarsal hesaplama matrisli kalibrasyon (MC) ile yapılmıştır. Analiz metodunun validasyonu, geri alım, metot dedeksiyon limiti, tekrar edilebilirlik, kesinlik gibi metot performans kriterleri ile gerçekleştirilmiş ve tüm değerler olması gereken limitler içinde bulunmuştur. Her iki elma çeşidi için imidacloprid ve dimethoate geri alım değeri ortalaması %88.34 (RSD %7.72) olarak tespit edilmiştir. Tüm metodun geri alımı ise %89.50 (RSD %12.02) olarak bulunmuştur (n = 150). Bu rakamlar olması gereken ortalama geri alım (%70-120) ve tekrar edilebilirlik (RSD

Method Validation for Imidacloprid and Dimethoate Residues in Apples by QuEChERS and LC-MS/MS Analysis.

Method Validation for Imidacloprid and Dimethoate Residues in Apples by QuEChERS and LC-MS/MS Analysis. All methods used for pesticide residue analysis must be validated prior to implementation of original laboratory samples analysis.This study performed to validate analytical procedure for imidacloprid ve dimethoate residues in apples. For this aim, untreated blank Golden Delicious and Starking Delicious samples were homogenized and fortified at 3 levels with pesticides. 10 g of apples were subjected to QuEChERS extraction and cleanup procedure. Pesticide analysis performed with LC-MS/MS. Since matrix effect was important for both pesticides and both apple varieties, matrix matched calibration (MC) was used for quantification. Method validation was carried out by performance parameters such as, recovery, method detection limit, repeatability, precision. All parameters figures were within the required limits. For imidacloprid and dimethoate analytes, recoveries (n=150) averaged 88.34% (RSD 7.72%), for two apple commodites over the validation range. For overall recovery of the analytical procedure was 89.50%(RSD12.02% ). These values were compatible with the required figure for recovery (70-120%) and repeatability (RSD

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