Validation of QuEChERS Based LC-MS/MS Determination Method for The Analysis of Some Neonicotinoid Insecticide Residues in Tomato Samples

Abstract

In this study, we aimed to validate the analytical procedure for the multiple residue analysis of imidacloprid, acetamiprid, thiamethoxam, clothianidin and thiacloprid in tomatoes. For this purpose, tomato samples were extracted and cleaned-up by using QuEChERS method. Chromatographic analyses were performed with LC-MS/MS. The method was validated according to the limit of detection (LOD), linearity, accuracy and recovery The linearity of five pesticides were determined with the range of 5-150 μg L-1. The correlation coefficients (r2) range from 0.992 to 0.996. The LODs were between 1.03 and 1.22 μg kg-1. The limits of quantification (LOQ) varied between 3.44 and 4.07 μg kg-1. The recovery of fortified tomato samples in five different neonicotinoid groups of insecticides at two different concentrations (10 μg kg-1, 50 μg kg-1) were conducted. For repeatability, the relative standard deviation (RSD%) ranged from 0.84 to 5.43, and for reproducibility, RSD% ranged from 4.58 to 15.15. The overall recovery of the method was 102.52% and the RSD was 9.79% (n = 300). All results were compatible with the values specified in SANTE (2017) for recovery (70–120%) and repeatability (RSD% ≤ 20%).

Keywords

• LC-MS/MS
• method validation
• neonicotinoid
• pesticide residue
• QuEChERS

Domates Numunelerinde Bazı Neonicotinoid Grubu İnsektisit Kalıntılarının Saptanmasında QuEChERS ve LC-MS/MS Metodunun Validasyonu

Öz

Yapılan bu çalışmada, domateste imidacloprid, acetamiprid, thiamethoxam, clothianidin ve thiacloprid çoklu kalıntı analizi için analiz prosedürünün valide edilmesi amaçlanmıştır. Bu amaçla domates örnekleri QuEChERS yöntemi ile ekstrakte edilerek LC-MS/MS cihazında analiz edilmiştir. Metot; tespit ve ölçüm limiti, doğrusallık ve doğruluk (tekrarlanabilirlik, tekrar üretilebilirlik, geri kazanma) limitine göre değerlendirilmiştir. Yöntemde beş pestisit için 5-150 μg L-1 aralığında doğrusallık saptanmıştır. Korelasyon katsayıları 0.992- 0.996, tespit limitleri (LOD) ise 1.03 ve 1.22 μg kg-1 arasında belirlenmiştir. Ölçüm limiti (LOQ) 3.44 ve 4.07 μg kg-1 arasındadır. Geri alım çalışmaları için domates örnekleri beş neonikotinoid grubu insektisit ile iki farklı konsantrasyon (10 μg kg-1, 50 μg kg-1) seviyesinde zenginleştirilmiştir. Tekrarlanabilirlik için, relatif standart sapma (RSD%) 0.84 ile 5.43 arasında, tekrar üretilebilirlik için (RSD%), 4.58 ile 15.15 arasında değişmiştir. Tüm metodun geri alımı %102.52, RSD ise %9.79 olarak bulunmuştur (n=300). Tüm bulgular SANTE (2017) 'de belirtilen geri alım sınırlarına (%70-120) ve kesinlik kabul oranı için belirtilen değerlere (%RSD ≤ %20) uygundur.

Anahtar Kelimeler

• LC-MS/MS
• metod validasyonu
• neonicotinoid
• pestisit kalıntısı
• QuEChERS

Kaynakça

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