Araştırma Makalesi
BibTex RIS Kaynak Göster

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

Yıl 2017, Cilt: 5 Sayı: 1, 29 - 37, 01.08.2017

Öz

Pestisit kalıntı
analizlerinde kullanılan tüm metotların, orijinal laboratuvar örneklerinin
analizinden önce validasyonu yapılmalıdır. Bu çalışmada elmalarda
imidacloprid
ve dimethoate kalıntı analizi için analiz prosedürünü 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. Sonra
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 tümü olması gereken limitler içinde bulunmuştur.
Her iki elma çeşiti için imidacloprid ve dimethoate
geri alım değeri ortalaması %88.34 (RSD %7.72) olarak bulunmuştur. 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 ≤ %20) değerleri ile
uyumludur
. Pestisitlerin
metot dedeksiyon limiti,  AB ve Türk Gıda
Kodeksi MRL değerlerinden düşük bulunmuştur. Her iki pestisit için kalibrasyon eğrisi
5–200 ng/mL konsantrasyon
sınırlarında doğrusal bulunmuştur.

Kaynakça

  • An, E.M., Shin, H.S., 2011. Gas Chromatographic Determination of Pesticide Residues Using Electron-capture Detector and Mass Spectrometry. Food Science and Biotechnology, 20 (5):1299-1306.
  • Anastassiades, M., Lehotay, S.J., Stajnbaher, D., Schenck, F.J., 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
  • Anonymous, 2002. Community Methods of Sampling for The Official Control of Pesticide Residues in and on Products of Plant and Animal Origin and Repealing. Commission Directive 79/700/EEC.
  • Aysal, P., Ambrus, A,R., Lehotay, S, J., 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.
  • Ellison, S. L. R., 2006. In Defence of Correlation Coefficient. Accreditation and Quality Ass., (11): 146-152.
  • Gonzales, A.G., Herrador, M.A., Asuero, A.G., Sayago, A., 2006. The Correlation Coefficient Attack Again. Accreditation and Quality Assurance, (11): 256-258.
  • Huber, W., 2004. On the Use of Correlation Coefficient for Testing the Linearity of Calibration Function. Accreditation and Quality Assurance, 9:726.
  • Kanrar, B., Mandal, S., Bhattacharyya, A., 2010. Validation and Uncertainty Analysis of A Multi Residue Method for 42 Pesticides in Made Tea. J. of Chromatography A, 1217:1926–1933.
  • Lehotay, S. J., Maśtovská, K., Lightfield, A. R., 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 International. 88(2): 615-629.
  • Lemes, V.R.R, Martins-Júnior, H.A., Souza, S.V.C., Colacioppo, S., 2014. Ethylenethiourea in Fruits: Optimization and in-House Validation of a Method by Liquid Chromatography Tandem Mass Spectrometry, Occurrence and Dietary Exposure Assessment. Food Control. 42:321–328.
  • Lesueur, C., Knıttl, P., Gartner, M., Mentler, A., Fuerhacker, M., 2008. Analysis Of 140 Pesticides from Conventional Farming Foodstuff Samples After Extraction with the Modified QuECheRS Method, Food Control, 19:906-914.
  • Miller, J.N., Ambrus, A., 2005. Significance Test 1, Statistics in Calibration Analysis, I and II. Manual on Basic Statistics. In Lectures Database, FAO/IAEAWorkshop on Introduction to QC/QA Measures in Pesticide Residue Analytical Laboratories, Seibersdorf, Vienna, Austria.
  • SANCO, 2013. Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. 2013, Document No. SANCO/12571/2013 http://www.eurl-pesticides.eu/library/docs/allcrl/ AqcGuidance_Sanco_2013_12571.pdf Erişim:13.05.2014).
  • Singh, S.B., Foster, G.D., Khan, S.U., 2007. Determination of Thiophanate Methyl and Carbendazim Residues in Vegetable Samples Using Microwave-Assisted Extraction. J. of Chromatography A, 1148:152–157.
  • Temur, C., Tiryaki, O., Uzun, O., Başaran, M. 2012. Adaptation and validation of QuEChERS method fort he analysis of Trifluralin in wind-eroded soil. J of Environmental Science and Health Part B, 47, 842-850.
  • Thompson, M., Ellison, S.L.R., Wood, R.., 2002. Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis. Pure and Applied Chemistry,74(5): 835–855.
  • Tiryaki, O., 2006. Method validation for the analysis of pesticide residues in grain by thin-layer chromatography. Accreditation and Quality Assurance, 11(10):506-514.
  • Tiryaki, O., 2011. Pestisit Kalıntı Analizlerinde Kalite Kontrol (QC) ve Kalite Güvencesi (QA) Nobel Yayın No: 1635, Fen Bilimleri: 116, Nobel Bilim ve Araştırma Merkezi Yayın No:73.
  • Tiryaki, O., Baysoyu, D., 2006. Estimation of sample processing uncertainty for Chlorpyrifos Residue in Cucumber. Accreditation and Quality Assurance, 10 (10): 550-553.
Yıl 2017, Cilt: 5 Sayı: 1, 29 - 37, 01.08.2017

Öz

Kaynakça

  • An, E.M., Shin, H.S., 2011. Gas Chromatographic Determination of Pesticide Residues Using Electron-capture Detector and Mass Spectrometry. Food Science and Biotechnology, 20 (5):1299-1306.
  • Anastassiades, M., Lehotay, S.J., Stajnbaher, D., Schenck, F.J., 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
  • Anonymous, 2002. Community Methods of Sampling for The Official Control of Pesticide Residues in and on Products of Plant and Animal Origin and Repealing. Commission Directive 79/700/EEC.
  • Aysal, P., Ambrus, A,R., Lehotay, S, J., 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.
  • Ellison, S. L. R., 2006. In Defence of Correlation Coefficient. Accreditation and Quality Ass., (11): 146-152.
  • Gonzales, A.G., Herrador, M.A., Asuero, A.G., Sayago, A., 2006. The Correlation Coefficient Attack Again. Accreditation and Quality Assurance, (11): 256-258.
  • Huber, W., 2004. On the Use of Correlation Coefficient for Testing the Linearity of Calibration Function. Accreditation and Quality Assurance, 9:726.
  • Kanrar, B., Mandal, S., Bhattacharyya, A., 2010. Validation and Uncertainty Analysis of A Multi Residue Method for 42 Pesticides in Made Tea. J. of Chromatography A, 1217:1926–1933.
  • Lehotay, S. J., Maśtovská, K., Lightfield, A. R., 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 International. 88(2): 615-629.
  • Lemes, V.R.R, Martins-Júnior, H.A., Souza, S.V.C., Colacioppo, S., 2014. Ethylenethiourea in Fruits: Optimization and in-House Validation of a Method by Liquid Chromatography Tandem Mass Spectrometry, Occurrence and Dietary Exposure Assessment. Food Control. 42:321–328.
  • Lesueur, C., Knıttl, P., Gartner, M., Mentler, A., Fuerhacker, M., 2008. Analysis Of 140 Pesticides from Conventional Farming Foodstuff Samples After Extraction with the Modified QuECheRS Method, Food Control, 19:906-914.
  • Miller, J.N., Ambrus, A., 2005. Significance Test 1, Statistics in Calibration Analysis, I and II. Manual on Basic Statistics. In Lectures Database, FAO/IAEAWorkshop on Introduction to QC/QA Measures in Pesticide Residue Analytical Laboratories, Seibersdorf, Vienna, Austria.
  • SANCO, 2013. Guidance document on analytical quality control and validation procedures for pesticide residues analysis in food and feed. 2013, Document No. SANCO/12571/2013 http://www.eurl-pesticides.eu/library/docs/allcrl/ AqcGuidance_Sanco_2013_12571.pdf Erişim:13.05.2014).
  • Singh, S.B., Foster, G.D., Khan, S.U., 2007. Determination of Thiophanate Methyl and Carbendazim Residues in Vegetable Samples Using Microwave-Assisted Extraction. J. of Chromatography A, 1148:152–157.
  • Temur, C., Tiryaki, O., Uzun, O., Başaran, M. 2012. Adaptation and validation of QuEChERS method fort he analysis of Trifluralin in wind-eroded soil. J of Environmental Science and Health Part B, 47, 842-850.
  • Thompson, M., Ellison, S.L.R., Wood, R.., 2002. Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis. Pure and Applied Chemistry,74(5): 835–855.
  • Tiryaki, O., 2006. Method validation for the analysis of pesticide residues in grain by thin-layer chromatography. Accreditation and Quality Assurance, 11(10):506-514.
  • Tiryaki, O., 2011. Pestisit Kalıntı Analizlerinde Kalite Kontrol (QC) ve Kalite Güvencesi (QA) Nobel Yayın No: 1635, Fen Bilimleri: 116, Nobel Bilim ve Araştırma Merkezi Yayın No:73.
  • Tiryaki, O., Baysoyu, D., 2006. Estimation of sample processing uncertainty for Chlorpyrifos Residue in Cucumber. Accreditation and Quality Assurance, 10 (10): 550-553.
Toplam 19 adet kaynakça vardır.

Ayrıntılar

Konular Ziraat Mühendisliği
Bölüm Makaleler
Yazarlar

Osman Tiryaki

Ezgi Özel

Yayımlanma Tarihi 1 Ağustos 2017
Yayımlandığı Sayı Yıl 2017 Cilt: 5 Sayı: 1

Kaynak Göster

APA Tiryaki, O., & Özel, E. (2017). Elmalarda İmidacloprid ve Dimethoate Kalıntıları için QuEChERS ve LC–MS/MS ile Metot Validasyonu. ÇOMÜ Ziraat Fakültesi Dergisi, 5(1), 29-37.