Sıvı Kromatografi-Tandem Kütle Spektrometrisi ile Modifiye QuEChERS Yöntemi Kullanılarak Chlorsulfuron ve Pendimethalinin Toprakda Belirlenmesi

Öz

Ekosistemde yüksek konsantrasyonlarda biriken pestisitler, canlıların besin zincirine karışarak onlara önemli zararlar vermektedir. Pestisitlerin yaygın kullanımı nedeniyle toprak ve su kirliliğinin sürekli artması, pestisitlerin tespiti için etkin analitik yöntemlerin geliştirilmesini ve bu yöntemlerle kalıntı düzeylerinin sürekli izlenmesini gerekli kılmıştır. Bu çalışmada, toprak matrisinde chlorsulfuron ve pendimenthalin tespiti için analitik bir yöntem geliştirilmiş ve valide edilmiştir. Toprak numunesi bilinen miktarda pestisit ile üç farklı konsantrasyonda (0.01, 0.05 ve 0.1 mg/kg) fortifike edilmiş ve analitler modifiye QuEChERS yöntemi ile ekstrakte edilmiştir. Geri kazanım çalışmaları 5 farklı modifiye QuEChERS yöntemi ile gerçekleştirilmiştir. T4 yönteminde (266.6 mg MgSO4, 66.6 mg NaCl, 66.6 mg TSCD ve 33.3 mg DHS ile ekstraksiyon, 300 mg MgSO4 ve 100 mg PSA ile d-SPE temizliği) daha iyi geri kazanımlar elde edilmiştir. Geri kazanımlar %70-120 aralığında olup, bağıl standart sapma (RSD) değerleri %15'ten düşük bulunmuştur. Chlorsulfuron ve pendimenthalin sırasıyla LOD değerleri 0,96 ve 1,30 μg kg-1 ve LOQ değerleri 3,19 ve 4,34 μg kg-1 olarak belirlenmiştir.

Anahtar Kelimeler

• dSPE
• LC-MS/MS
• Metod validasyonu
• Pestisit kalıntısı
• Toprak

Determination of Chlorsulfuron and Pendimethalin in Soil Samples Using Modified QuEChERS Method by Liquid Chromatography-Tandem Mass Spectrometry

Abstract

Pesticides, which accumulate in the ecosystem at high concentrations, interfere with the food chain of life forms and cause significant damage to them. The continuous increase in soil and water pollution due to the extensive use of pesticides has made it necessary to develop effective analytical methods to detect pesticides and to continuously monitor the level of residues with these methods. In this study, an analytical method for the detection of chlorsulfuron and pendimenthalin in soil matrix was developed and validated. The soil sample was fortified with a known quantity of pesticides at three different concentration levels (0.01, 0.05 and 0.1 mg/kg) and the analytes were extracted via a modified QuEChERS method. Recovery studies were performed with 5 different modified QuEChERS methods. Better recoveries were obtained in T4 method (extraction with 266.6 mg MgSO4, 66.6 mg NaCl, 66.6 mg TSCD and 33.3 mg DHS, d-SPE cleanup with 300 mg MgSO4 and 100 mg PSA). The recoveries were in the range 70–120 %, with relative standard deviation (RSD)values lower than 15 %. Chlorsulfuron and pendimenthalin of Limits of detection (LODs) were 0.96 and 1.30 μg kg−1 and limits of quantification (LOQs) were 3.19 and 4.34 μg kg−1, respectively.

Keywords

• dSPE
• LC-MS/MS
• Method validation
• Pesticide residue
• Soil

Kaynakça

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