Bitki koruma ürünlerinin kalıntı analizlerinde temel laboratuvar işlemlerinin ölçüm belirsizlikleri

Bitki koruma ürünlerinin (pestisit) kalıntı analizlerinde, analiz sonuçlarının güvenirliği kalite güvence(QA) ve kalite kontrol(QC) parametreleri ile ispatlanmalıdır. Bu parametrelerden en önemlilerinden biri de laboratuvardaki işlemlerin ölçüm belirsizliğidir. “Uluslararası Standart Organizasyonu (ISO) 17025”, “ISO Ölçüm Belirsizliği Açıklama Kılavuzu (GUM)” ve “EUREACHEM/CITAC Guide CG4” gibi uluslararası dokümanlara göre, temel laboratuvar işlemlerinin belirsizliklerinin ölçülmesi bir zorunluluktur. Analizlerdeki ölçümler her zaman tam ve kesin değildir ve bu kesin olmamanın (belirsizliklerin) derecesinin rakamsal olarak ifade edilmesi gerekir. Ölçüm belirsizliği bir ölçümün sonucu ile ilgili olası dalgalanmaları tanımlayan istatistiksel parametredir. Analizle ilgili her bir laboratuvar islemlerinin ve prosedurlerinin belirsizliğinin saptanarak ve daha sonra da birlestirilmis toplam belirsizlik hesaplanması ile bulunabilir. Bu makale, güncel literatür taranarak, analiz islemlerine girmeden, isin baslangıcında, basit fakat etkisi önemli olan tartımsal ve hacimsel işlemler ile bunlarla ilgili diğer bazı temel laboratuvar islemlerinin belirsizliğinin “bireyselden-tüme” yaklaşımı ile saptanması ile ilgilidir.

Uncertainty measurement of basic laboratory operations in the residue analysis of plant protection products

In residue analysis of plant protection products (pesticide), the reliability of analytical results have to be proved with the quality assurance (QA) and quality control (QC) parameters. One of the most important of these parameters is the uncertainty in the measurement of basic laboratory operations. According to documents like“International Organisation for Standardisation (ISO) 17025”, “ISO Guide to the Expression of Uncertainty in Measurement (GUM)”, and “EUREACHEM/CITAC Guide CG4” (A Focus for Analytical Chemistry in Europe/The Cooperation on International Traceability in Analytical Chemistry), the uncertainty of measurements in basic laboratory operations should be estimated. Measurement results in the laboratory are not always certain, and the degree of these uncertainties have to be figured out numerically Measurement uncertainty is a statistical parameter which describes the possible fluctations of a measurement results. It can be determined by the estimation uncertainty of individual components of any operation and test procedure, and later by the calculations of combined total uncertainty. Basing on uptodate references, this article deals, without touching analytical operations, with the estimation of uncertainty of basic laboratory operations such as weighing and volumetric equipment, and some other related operations, by using “bottom-up” approaches.

___

  • Anonymous, 1986. CRC Handbook of chemistry and physics 67th Edition F-4, F-5 CRC Press.
  • Anonymous, 1995. Guide to the Expression of Uncertainty in Measurement, ISO, Geneva, 1995, ISBN92-67-10188-9. (Reprinted 1995).
  • Anonymous 2000. EURACHEM/CITAC Guide CG 4. Quantifying Uncertainty in Analytical Measurements, 2nd Edtn. (QUAM:2000.P1) http://www. measurementuncertainty. org/mu /QUAM2000-1.pdf (Ulasım: 07.04.2008).
  • Anonymous, 2004. ISO/TS 21748, Guidance for the Use of Repeatability, Reproducibility and Trueness Estimates in Measurement, 2004.
  • Anonymous, 2005. EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories, CEN Management Centre, Brussels.
  • Anonymous, 2006. Quality control procedures for pesticide residue analysis, Document No SANCO/10232/ 2006, 24/March/2006.
  • Anonymous, 2007a. Joint Comittee fr Guides in Metrology , International vocabulary of basic ande general terms in metrology(ISO), VIM3,Geneva, third ed.
  • Anonymous 2007b. European Ccommission DG SANCO, Method validation and quality control procedures for pesticide residue analysisin food and feed, No SANCO/2007/3131/31 October 2007.
  • Barwick, V.J., 1998. VAM Project 3.2.2 Evaluating Confidence in Analytical Measurement. Part (a): Literature review of uncertainty in laboratory operations. Review of sources of uncertainty in gas chromatography and high performance liquid chromatography. LGC/VAM/1998/053. Setting standards in analytical science.
  • Benyhe, J., 1998. Testing the uncertainty of laboratory operations. In Pesticide residue analysis/Laboratory exercises “FAO/IAEA/SIDA Training Workshop on the "Quality Assurance and Quality Control Measures in Residue Analysis Laboratories” 2 March - 27 March Training and Reference Center for Food and Pesticide Control, Miskolc, Hungary.
  • De Bièvre, P., 2007. The beginning of the end of the confusion in concepts and terms? The new international vocabulary of basic and general concepts in metrology (VIM). Accred. Qual. Assur., 12: 279-281.
  • Hibbert, D.B., 2007. Systematic errors in analytical measurement results. J. Chromatogr A., 1158: 25- 32.
  • Maestroni, M.B., 2005. Uncertainty of laboratory operations. In Lectures Database/Uncertainty of analytical results/Principles of estimation of uncertainty. FAO/IAEA Training Workshop on Introduction to QC/QA in Pesticide Analytical Laboratories, Training and Reference Center for Food and Pesticide Control, Seibersdorf, Vienna, Austria, 12 Sept- 7Oct 2005.
  • Meyer, V.R., 2007. Measurement uncertainty. J. Chromatography A., 1158: 15-24.
  • Shegunova, P., Bercaru, O., Olsen, B.S., 2008. Estimation of measurement uncertanty in organic analysid: two practical approaches. Accred. Qual. Assur., 13(1):11-18.
  • Stepan, R., Hajšlová, J., Kocourek, V., Tichá, J., 2004. Uncertainties of gas chromatographic measurement of troublesome pesticide residues in apples employing conventional and mass spectrometric detectors. Analytica Chimica Acta, 520: 245-255.
  • Tiryaki, O., Baysoyu, D., 2007. The Use of Radiotracer Techniques for QA/QC Principles in Pesticide Residue Analysis. Ankara Üniversitesi Ziraat Fakültesi, Tarım Bilimleri Dergisi, 13 (2):108-113.
  • Tiryaki, O., Baysoyu, D., 2008. Estimation of efficiencies and uncertainties of the extraction and cleanup steps of the pesticide residue determination in cucumber using 14C-carbaryl. Accred. Qual. Assur., 13(2):91-99.
  • Vanatta, L.E., Coleman, D.E., 2007. Calibration, uncertainty, and recovery in the chromatographic sciences. J. Chromatogr A, 1158: 47-60.
  • Visi, E., 2002. Quality Assurance/Quality Control in pesticide residue laboratories. Possibilities of controlling the various analytical steps. FAO/IAEA Training and Reference Centre for Food and Pesticide Control Training workshop on Introduction to QC/QA measures in Pesticide Residue Analytical Lab. 17 June - 26 July IAEA’s Laboratories Seibersdorf; Austria.