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Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu

Year 2018, Volume: 4 Issue: 2, 33 - 45, 17.12.2018
https://doi.org/10.28979/comufbed.410403

Abstract

QuEChERS metodu ile “Golden Delicious” ve “Starking Delicious” elma çeşitlerinde chlorpyrifos etken maddenin kalıntı analizi için 0.05, 0.5 ve 5.0 mg/kg seviyelerinde zenginleştirme yapılarak validasyon gerçekleştirilmiştir. Analizler yapıldıktan sonra LC-MS/MS kullanılarak kromatografik ayrıştırma yapılmıştır. Matris etkisini elimine etmek için matrisli kalibrasyon (MC) kullanılmıştır. Bu yüzden, MCGolden D ve MCStarking D kalibrasyonları kullanılmıştır. Metodun validasyonu, gerçeğe yakınlık (accuracy), kalibrasyonun doğrusallığı, geri alım, cihaz dedeksiyon limiti, metodun tespit limiti, tekrar edilebilirlik ve kesinlik gibi kriterler ile gerçekleştirilmiştir. Her iki çözücü kalibrasyon kurvesi ve her iki matris kalibrasyon eğrisi 5-200 pg/µl aralığında lineer olarak bulunmuştur. Golden D örneğinden geri alımı; %8.36-14.03 tekrar edebilirlik değerleri ile %70.87-112.99 arasında bulunmuştur (ortalama geri alım %89.32). Starking D elma örneği için ise geri alım; %1.96-12.88 tekrar edebilirlik değerleri ile  %69.08-100.3 arasında bulunmuştur (ortalama geri alım %79.82). Tüm metodun geri alımı %15.68 relatif standart sapma ile  %84.60 olarak bulunmuştur. Tüm bulgular olması gereken geri alım sınırlarına (%70-120) ve tekrar edebilirlik kabul oranı için belirtilen değerlere (RSD ≤% 20) uygundur.

References

  • Aksu P., 2007. Meyve ve Sebzelerdeki Pestisit Kalıntılarının Tayininde Gaz Kromatografisi/ Kütle Spektrometresi (GC/MS) ile Çoklu Kalıntı Analiz Yönteminin Geliştirilmesi. s:379. Ambrus A., 2004. Reliability of Measurements of Pesticide Residues in Food. Accreditation Quality Assurance, 9: 288-304.
  • 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.
  • Anonim, 1999. AOAC/FAO/IAEA/IUPAC., Guidelines for Single-laboratory Validation of Analytical Methods for Trace-level Concentrations of Organic Chemicals Expert Consultation Meeting, Miskolc, Hungary. 21 February 2016, http://www.iaea.org/trc/pest-qa_val_ guide.pdf.
  • Anonim, 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. https://www.fsvps.ru/fsvps-docs/ru/usefulinf/files/es2002-63.pdf
  • Anonim, 2016. Aydın Gıda Tarım ve Hayvancılık İl Müdürlüğü. http://aydin.tarim.gov.tr/Duyuru/138/ Bakanligimizca-Chlorpyrifos-Ethyl-Aktif-Maddesi-Iceren-Urunler-Yasaklandi. Ersişim: 01.06.2016
  • Aysal P., Ambrus A., 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.
  • Durmaz, 2016. Elmalarda QuEChERS Yöntemi ile Chlorpyrifos Analizi İçin Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi, (Basılmamış), Yüksek Lisans tezi,s.52 Ellison S., L. R., 2006. In Defence of Correlation Coefficient. Accred. and Qual. Assurance, 11: 146-152.
  • Gonzales A.G., Herrador M.A., Asuero A.G., Sayago A., 2006. The Correlation Coefficient Attack Again. Accred. and Qual. Assurance, (11): 256-258.
  • Huber W., 2004. On the Use of Correlation Coefficient for Testing the Linearity of Calibration Function. Accred. and Qual. 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. Journal 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.
  • 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.
  • SANTE, 2017. Guidance document on analytical quality control and method validation pro-cedures 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.
  • Rashid A., Nawaz S., Barker H., Ahmad I., Ashraf M., 2010. Development of a Simple Extraction and Clean-Up Procedure for Determination of Organochlorine Pesticides in Soil Using Gas Chromatographytandem Mass Spectrometry. Journal of Chromatography A 1217: 2933–2939.
  • Singh S.B., Foster G.D., Khan S.U., 2007. Determination of Thiophanate Methyl and Carbendazim Residues in Vegetable Samples Using Microwave-Assisted Extraction. Journal of Chromatography A 1148: 152–157.
  • 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., Baysoyu D., 2006. Estimation of Sample Processing Uncertainty for Chlorpyrifos Residue in Cucumber. Accreditation and Quality Assurance 10 (10): 550-553.
  • 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.
  • Vryzas Z., Myresiotis C., Papadakis E., . Kyrgidou A., Papadopoulou- Mourkidou E., 2008. Tobacco Matrix Effect in Carbamate Residues Analysis. Annual Conference of the Mediterranean Group of Pesticide Residue (MGPR); Chemicals and their Residues in Food and Water: New Scenarios of the Modern Sustainable Agricultural Production, Proceedings Book, Piacenza-Italy. 58 p.

Method Validation for the Chlorpyrifos in Apples by QuEChERS Analysis Method

Year 2018, Volume: 4 Issue: 2, 33 - 45, 17.12.2018
https://doi.org/10.28979/comufbed.410403

Abstract

QuEChERS method was validated using “Golden Delicious ’’ and “Starking Delicious” apples, fortified with 0.05, 0.5 and 5.0 µg/g chlorpyrifos. Analyses were performed by QuEChERS method then chromatographic separation was performed by using LC-MS/MS. Calibration with matrix (MC) was used to compensate matrix effect. Thus MCGolden D and MCStarking D were used for quantification. The method validated by using following parameters; accuracy, linearity of calibration, recovery, instrument detection limit, estimated method detection limit, repeatability and precision. Calibration curve of solvent and both matrix matched calibration curve were the linear over the range of 5–200 pg/µl. Recovery of chlorpyrifos from Golden D apples were between 70.87–112.99% (mean recovery 89.32%) with the repeatability of 8.36-14.03%. Similarly recovered chlorpyrifos from Starking D apples ranged between 69.08–100.3% (mean recovery 79.82%) with the repeatability of 1.96-12.88%. For overall recovery of the procedure was 84.60% ( RSD= 15.68%). These all figures comply with the determined values for average recovery limits (70-120%) and precision (RSD ≤ 20%).

References

  • Aksu P., 2007. Meyve ve Sebzelerdeki Pestisit Kalıntılarının Tayininde Gaz Kromatografisi/ Kütle Spektrometresi (GC/MS) ile Çoklu Kalıntı Analiz Yönteminin Geliştirilmesi. s:379. Ambrus A., 2004. Reliability of Measurements of Pesticide Residues in Food. Accreditation Quality Assurance, 9: 288-304.
  • 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.
  • Anonim, 1999. AOAC/FAO/IAEA/IUPAC., Guidelines for Single-laboratory Validation of Analytical Methods for Trace-level Concentrations of Organic Chemicals Expert Consultation Meeting, Miskolc, Hungary. 21 February 2016, http://www.iaea.org/trc/pest-qa_val_ guide.pdf.
  • Anonim, 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. https://www.fsvps.ru/fsvps-docs/ru/usefulinf/files/es2002-63.pdf
  • Anonim, 2016. Aydın Gıda Tarım ve Hayvancılık İl Müdürlüğü. http://aydin.tarim.gov.tr/Duyuru/138/ Bakanligimizca-Chlorpyrifos-Ethyl-Aktif-Maddesi-Iceren-Urunler-Yasaklandi. Ersişim: 01.06.2016
  • Aysal P., Ambrus A., 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.
  • Durmaz, 2016. Elmalarda QuEChERS Yöntemi ile Chlorpyrifos Analizi İçin Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi, (Basılmamış), Yüksek Lisans tezi,s.52 Ellison S., L. R., 2006. In Defence of Correlation Coefficient. Accred. and Qual. Assurance, 11: 146-152.
  • Gonzales A.G., Herrador M.A., Asuero A.G., Sayago A., 2006. The Correlation Coefficient Attack Again. Accred. and Qual. Assurance, (11): 256-258.
  • Huber W., 2004. On the Use of Correlation Coefficient for Testing the Linearity of Calibration Function. Accred. and Qual. 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. Journal 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.
  • 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.
  • SANTE, 2017. Guidance document on analytical quality control and method validation pro-cedures 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.
  • Rashid A., Nawaz S., Barker H., Ahmad I., Ashraf M., 2010. Development of a Simple Extraction and Clean-Up Procedure for Determination of Organochlorine Pesticides in Soil Using Gas Chromatographytandem Mass Spectrometry. Journal of Chromatography A 1217: 2933–2939.
  • Singh S.B., Foster G.D., Khan S.U., 2007. Determination of Thiophanate Methyl and Carbendazim Residues in Vegetable Samples Using Microwave-Assisted Extraction. Journal of Chromatography A 1148: 152–157.
  • 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., Baysoyu D., 2006. Estimation of Sample Processing Uncertainty for Chlorpyrifos Residue in Cucumber. Accreditation and Quality Assurance 10 (10): 550-553.
  • 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.
  • Vryzas Z., Myresiotis C., Papadakis E., . Kyrgidou A., Papadopoulou- Mourkidou E., 2008. Tobacco Matrix Effect in Carbamate Residues Analysis. Annual Conference of the Mediterranean Group of Pesticide Residue (MGPR); Chemicals and their Residues in Food and Water: New Scenarios of the Modern Sustainable Agricultural Production, Proceedings Book, Piacenza-Italy. 58 p.
There are 22 citations in total.

Details

Primary Language Turkish
Subjects Engineering
Journal Section Araştırma Makalesi
Authors

Ahmet Durmaz This is me

Osman Tiryaki

Publication Date December 17, 2018
Acceptance Date September 7, 2018
Published in Issue Year 2018 Volume: 4 Issue: 2

Cite

APA Durmaz, A., & Tiryaki, O. (2018). Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, 4(2), 33-45. https://doi.org/10.28979/comufbed.410403
AMA Durmaz A, Tiryaki O. Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi. December 2018;4(2):33-45. doi:10.28979/comufbed.410403
Chicago Durmaz, Ahmet, and Osman Tiryaki. “Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi Ile Metot Validasyonu”. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi 4, no. 2 (December 2018): 33-45. https://doi.org/10.28979/comufbed.410403.
EndNote Durmaz A, Tiryaki O (December 1, 2018) Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi 4 2 33–45.
IEEE A. Durmaz and O. Tiryaki, “Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu”, Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, vol. 4, no. 2, pp. 33–45, 2018, doi: 10.28979/comufbed.410403.
ISNAD Durmaz, Ahmet - Tiryaki, Osman. “Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi Ile Metot Validasyonu”. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi 4/2 (December 2018), 33-45. https://doi.org/10.28979/comufbed.410403.
JAMA Durmaz A, Tiryaki O. Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi. 2018;4:33–45.
MLA Durmaz, Ahmet and Osman Tiryaki. “Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi Ile Metot Validasyonu”. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi, vol. 4, no. 2, 2018, pp. 33-45, doi:10.28979/comufbed.410403.
Vancouver Durmaz A, Tiryaki O. Elmalarda Chlorpyrifos’un QuEChERS Analiz Yöntemi ile Metot Validasyonu. Çanakkale Onsekiz Mart Üniversitesi Fen Bilimleri Enstitüsü Dergisi. 2018;4(2):33-45.

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