Nektarin ve Şeftali Örneklerinde Bazı Pestisit Kalıntılarının Belirlenmesi İçin Etkin Bir Yöntemin Doğrulanması

Öz

Metot doğrulama, yöntemin belirli bir amaca uygunluğunu doğrulayan bir iç kalite kontrol prosedürüdür. Gerçek örneklerin analizinden önce tüm analiz metotları doğrulanmalıdır. Metot doğrulamasını gerçekleştirmek için LOQ, doğrusal aralık, kesinlik, doğruluk ve geri kazanım gibi kriterler dikkate alınmalıdır. Bu çalışma nektarin ve şeftalide boscalid, chlorpyrifos ve tebuconazole analizi için QuEChERS analiz prosedürünü doğrulamak amacıyla yapılmıştır. Nektarin ve şeftali örnekleri 3 farklı seviyede 3 pestisitle spike edilmiştir. Ekstraksiyon ve clean-up basamakları için QuEChERS yöntemi uygulanmuştır. Kromatografik ayrıştırma LC-MS/MS ile yapılmıştır. Matris etkisini elimine etmek için matrisli kalibrasyon (MC) kullanılmıştır. QuEChERS metodu-LC-MS/MS analiz sistemi, pestisitlerin LOQ'larının MRL'nin altında olduğunu göstermiştir. Chlorpyrifos, tebuconazole ve boscalid pestisitlerinin nektarin örneklerinden geri alımları, sırasıyla %108.1, %109.9, ve %124.5 olarak bulunmuştur. Bu değerler şeftali örnekleri için sırasıyla, %108.4, %109.9 ve %122.3 şeklinde olmuştur. Yöntemin tüm geri alımı nektarin için %113.6, şeftali %113.5 olmuştur. Bu değerler SANTE geri kazanım limitleri (%60–140) ile uyumludur. MC eğrileri 3 pestisit için de doğrusal (R2 ≤0.999) olarak bulunmuştur. Geri alım, kesinlik, doğruluk ve doğrusallık gibi bazı diğer yöntem doğrulama kriterleri gerekli aralıklarda bulunmuştur. Nektarin ve şeftali örneklerinde, chlorpyrifos, tebuconazole and boscalid kalıntılarının analizleri için QuEChERS yöntemi uygun bulunmuştur.

Anahtar Kelimeler

• Şeftali
• Nektarin
• Pestisit Kalıntısı
• Metot Doğrulama
• QuEChERS

Verification of An Efficient Method for the Determination of Some Pesticide Residues in Nectarine and Peach

Öz

Method verification is an internal quality control procedure verifying the suitability of the method for specific purposes. All methods should be verified prior to analyses of real samples. LOQ, range of linearity, precision, accuracy and recovery criteria have to be taken into consideration while performing the method verification. This study was conducted to verify QuEChERS procedure for the analysis of boscalid, chlorpyrifos and tebuconazole in nectarine and peach. Samples spiked at 3 levels of 3 different pesticides. LC-MS/MS was used for chromatographic separation. Matrix calibration (MC) was used to compensate the matrix effect. QuEChERS method revealed that all pesticide LOQs were less than MRL. Recovered boscalid, chlorpyrifos and tebuconazole from matrices were recorded as 123.73% (RSD= 8.89%; n=52), 108.37% (RSD= 14.95%; n=52) and 110.34% (RSD= 15.22%; n=52), respectively. Overall recovery of the QuEChERS-AOAC 2007.01 method was 113.96 %, with RSD value of 14.52 % (n=156; SD=16.55). All recovery ranges were noted as 66.42-139.68%. These values were fit the SANTE recovery ranges (60–140%). MC curves 3 pesticides were linear (R2 ≤0.999). Some other verification criteria, such as accuracy, linearity, precision and recovery were within the specified limits. According to the results of this study, the QuEChERS method is suitable for the analyses of chlorpyrifos, tebuconazole and boscalid in case of nectarine and peachs.

Anahtar Kelimeler

• : Peach
• Nectarine
• Pesticide Residues
• Method Verification
• QuEChERS

Kaynakça

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