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

Yıl 2020, Cilt: 37 Sayı: 1, 30 - 37, 30.04.2020
https://doi.org/10.13002/jafag4662

Öz

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%).

Kaynakça

  • Amadeo FA and Juan FGR (2008). Large-scalemulti-residue methods for pesticides and their degradation products in food by advanced LC-MS. Trac- Trend. Anal. Chem, 27: 973.
  • Anonymous (2016). Türk Gıda Kodeksi Pestisitlerin Maksimum Kalıntı Limitleri Yönetmeliği https://www.resmigazete.gov.tr/eskiler/2016/11/20161125M1-1.html (Accessed to web: 20.11.2019).
  • Anastassiades M, Lehotay SJ, Stajnbaher D and Schenck FJ (2003). Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid–phase extraction for the determination of pesticide residues in produce. Journal of AOAC International, 86: 412–431.
  • Aysal P, Ambrus AR, Lehotay SJ and Cannavan A (2007). Validation of an efficient method for the determination of pesticide residues in fruits and vegetables using ethyl acetate for extraction. Journal of Environmental Science and Health Part B, 42: 481–490.
  • Banerjee T, Gupta S, Singh B and Narayanan N (2019). LC-MS/MS method optimization and validation for trace-level analysis of 71 crop protection chemicals in pulses. Environ Monit Assess, 191: 670.
  • Bass C, Denholm I, Williamson MS and Nauen R (2015). The global status of insect resistance to neonicotinoid insecticides. Pesticide Biochemistry and Physiology, 121: 78-87.
  • Bayrak B (2018). Method Development and Validation for the Determination of Pesticide Residues in Water by GC-NPD. Iğdır Üni. Fen Bilimleri Enst. Der. / Iğdır Univ. J. Inst. Sci. & Tech, 8(1): 133-141.
  • Cimino AM, Boyles AL, Thayer KA and Perry MJ (2017). Effects of neonicotinoid pesticide exposure on human health: a systematic review. Environ Health Perspect, Feb;125(2): 155-162.
  • Dankyi E, Gordon C, Carboo D and Fomsgaard IS (2014). Quantification of neonicotinoid insecticide residues in soils from cocoa plantations using a QuEChERS extraction procedure and LC-MS/MS. Science of The Total Environment, 499: 276-283.
  • Durmaz A and Tiryaki O (2018). Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, 4(2): 33-45.
  • EC (2002). Commission Directive 2002/63/EC of 11 July 2002 Establishing Community Methods of Sampling for the Official Control of Pesticide Residues in and on Products of Plant and Animal Origin and Repealing. Directive 79/700/EEC. Offi. J. Euro. Comm., L 187/30, 1–14.
  • Ecobichon DJ (2001). Pesticide use in developing countries. Toxicology, 160(1-3):27-33.
  • Jeschke P, Nauen R, Schindler M and Elbert A (2011). Overview of the status and global strategy for neonicotinoids. J Agric Food Chem, 59: 2897-2908.
  • Lehotay SJ, Maśtovská K and Lightfield AR (2005). Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. Journal of AOAC Inter. 88(2):615-629.
  • Nauen R, Bielza P, Denholm I and Gorman K (2008). Age-specific expression of resistance to a neonicotinoid insecticide in the whitefly Bemisia tabaci. Pest Management Science, 64(11): 1106-1110.
  • Özel E and Tiryaki O (2017). Elmalarda İmidacloprid ve Dimethoate Kalıntıları için QuEChERS ve LC– MS/MS ile Metot Validasyonu. ÇOMÜ Zir. Fak. Derg. (COMU J. Agric. Fac.) 5(1).
  • Pietrzak D, Wątor K, Pękała D, Wójcik J, Chochorek A, Kmiecik E and Kania J (2019). LC-MS/MS method validation for determination of selected neonicotinoids in groundwater for the purpose of a column experiment, Journal of Environmental Science and Health, Part B, 54(5): 424-431.
  • Polat B and Tiryaki O (2019). Determination of some pesticide residues in conventional-grown and IPM-grown tomato by using QuEChERS method, Journal of Environmental Science and Health, Part B, 54(2):112-117.
  • Ramadan G, Jabir M, Alabdulmalik N and Mohammed A (2015). Validation of a method for the determination of 120 pesticide residues in apples and cucumbers by LC-MS/MS. Drug Test. Analysis, 8: 498- 510.
  • SANTE (2017). Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed (SANTE/11813/2017).https://ec.europa.eu/food/sites/food/files/plant/docs/pesticides_mrl_guidelines_wrkdoc_2017-11813.pdf (Accessed to web: 02.11.2019).
  • Suganthi A and Bhuvaneswari K (2018). Method Validation and Application of Liquid Chromatography- Mass Spectrometry/Mass Spectrometry for Determination of Neonicotinoid Pesticide Residues in Tomato. Journal of Chromatography Separation Techniques, 9(2).
  • Tiryaki O (2017). Pestisit Kalıntı Analizlerinde Kalite Kontrol (QC) ve Kalite Güvencesi (QA), Geliştirilmiş ve Güncelleştirilmiş 2. Basım. Nobel Yayın No: 1697, 274s, Ankara.

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

Yıl 2020, Cilt: 37 Sayı: 1, 30 - 37, 30.04.2020
https://doi.org/10.13002/jafag4662

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.

Kaynakça

  • Amadeo FA and Juan FGR (2008). Large-scalemulti-residue methods for pesticides and their degradation products in food by advanced LC-MS. Trac- Trend. Anal. Chem, 27: 973.
  • Anonymous (2016). Türk Gıda Kodeksi Pestisitlerin Maksimum Kalıntı Limitleri Yönetmeliği https://www.resmigazete.gov.tr/eskiler/2016/11/20161125M1-1.html (Accessed to web: 20.11.2019).
  • Anastassiades M, Lehotay SJ, Stajnbaher D and Schenck FJ (2003). Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid–phase extraction for the determination of pesticide residues in produce. Journal of AOAC International, 86: 412–431.
  • Aysal P, Ambrus AR, Lehotay SJ and Cannavan A (2007). Validation of an efficient method for the determination of pesticide residues in fruits and vegetables using ethyl acetate for extraction. Journal of Environmental Science and Health Part B, 42: 481–490.
  • Banerjee T, Gupta S, Singh B and Narayanan N (2019). LC-MS/MS method optimization and validation for trace-level analysis of 71 crop protection chemicals in pulses. Environ Monit Assess, 191: 670.
  • Bass C, Denholm I, Williamson MS and Nauen R (2015). The global status of insect resistance to neonicotinoid insecticides. Pesticide Biochemistry and Physiology, 121: 78-87.
  • Bayrak B (2018). Method Development and Validation for the Determination of Pesticide Residues in Water by GC-NPD. Iğdır Üni. Fen Bilimleri Enst. Der. / Iğdır Univ. J. Inst. Sci. & Tech, 8(1): 133-141.
  • Cimino AM, Boyles AL, Thayer KA and Perry MJ (2017). Effects of neonicotinoid pesticide exposure on human health: a systematic review. Environ Health Perspect, Feb;125(2): 155-162.
  • Dankyi E, Gordon C, Carboo D and Fomsgaard IS (2014). Quantification of neonicotinoid insecticide residues in soils from cocoa plantations using a QuEChERS extraction procedure and LC-MS/MS. Science of The Total Environment, 499: 276-283.
  • Durmaz A and Tiryaki O (2018). Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, 4(2): 33-45.
  • EC (2002). Commission Directive 2002/63/EC of 11 July 2002 Establishing Community Methods of Sampling for the Official Control of Pesticide Residues in and on Products of Plant and Animal Origin and Repealing. Directive 79/700/EEC. Offi. J. Euro. Comm., L 187/30, 1–14.
  • Ecobichon DJ (2001). Pesticide use in developing countries. Toxicology, 160(1-3):27-33.
  • Jeschke P, Nauen R, Schindler M and Elbert A (2011). Overview of the status and global strategy for neonicotinoids. J Agric Food Chem, 59: 2897-2908.
  • Lehotay SJ, Maśtovská K and Lightfield AR (2005). Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables. Journal of AOAC Inter. 88(2):615-629.
  • Nauen R, Bielza P, Denholm I and Gorman K (2008). Age-specific expression of resistance to a neonicotinoid insecticide in the whitefly Bemisia tabaci. Pest Management Science, 64(11): 1106-1110.
  • Özel E and Tiryaki O (2017). Elmalarda İmidacloprid ve Dimethoate Kalıntıları için QuEChERS ve LC– MS/MS ile Metot Validasyonu. ÇOMÜ Zir. Fak. Derg. (COMU J. Agric. Fac.) 5(1).
  • Pietrzak D, Wątor K, Pękała D, Wójcik J, Chochorek A, Kmiecik E and Kania J (2019). LC-MS/MS method validation for determination of selected neonicotinoids in groundwater for the purpose of a column experiment, Journal of Environmental Science and Health, Part B, 54(5): 424-431.
  • Polat B and Tiryaki O (2019). Determination of some pesticide residues in conventional-grown and IPM-grown tomato by using QuEChERS method, Journal of Environmental Science and Health, Part B, 54(2):112-117.
  • Ramadan G, Jabir M, Alabdulmalik N and Mohammed A (2015). Validation of a method for the determination of 120 pesticide residues in apples and cucumbers by LC-MS/MS. Drug Test. Analysis, 8: 498- 510.
  • SANTE (2017). Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed (SANTE/11813/2017).https://ec.europa.eu/food/sites/food/files/plant/docs/pesticides_mrl_guidelines_wrkdoc_2017-11813.pdf (Accessed to web: 02.11.2019).
  • Suganthi A and Bhuvaneswari K (2018). Method Validation and Application of Liquid Chromatography- Mass Spectrometry/Mass Spectrometry for Determination of Neonicotinoid Pesticide Residues in Tomato. Journal of Chromatography Separation Techniques, 9(2).
  • Tiryaki O (2017). Pestisit Kalıntı Analizlerinde Kalite Kontrol (QC) ve Kalite Güvencesi (QA), Geliştirilmiş ve Güncelleştirilmiş 2. Basım. Nobel Yayın No: 1697, 274s, Ankara.
Toplam 22 adet kaynakça vardır.

Ayrıntılar

Birincil Dil İngilizce
Bölüm Araştırma Makaleleri
Yazarlar

Tarık Balkan Bu kişi benim

Kenan Kara Bu kişi benim

Yayımlanma Tarihi 30 Nisan 2020
Yayımlandığı Sayı Yıl 2020 Cilt: 37 Sayı: 1

Kaynak Göster

APA Balkan, T., & Kara, K. (2020). Validation of QuEChERS Based LC-MS/MS Determination Method for The Analysis of Some Neonicotinoid Insecticide Residues in Tomato Samples. Journal of Agricultural Faculty of Gaziosmanpaşa University (JAFAG), 37(1), 30-37. https://doi.org/10.13002/jafag4662