Jakość wyników pomiarów analitycznych problemy i wyzwania

• Autorzy: Konieczka P.

Warianty tytułu

EN

Quality of analytical measurements problems and challenges

• Języki publikacji: PL

Abstrakty

PL

W pracy przedstawiono główne problemy związane z oceną, kontrolą i zapewnieniem jakości wyników pomiarów analitycznych. Podano charakterystykę poszczególnych elementów systemu jakości wyników pomiarów analitycznych wraz z omówieniem aktualnego stanu wiedzy dotyczącego spójności pomiarowej. szacowania niepew-ności wyników pomiaru, walidacji procedur analitycznych, stosowania materiałów odniesienia oraz wykorzystania i interpretacji wyników badań międzylaboratoryjnych. W pierwszej części pracy przedstawiono definicję podstawowych pojęć związanych z systemem kontroli jakości wyników pomiarów analitycznych oraz opisano sposoby i metody ich wyznaczania. Druga część pracy dotyczy osiągnięć autora w dziedzinie określania i wyznaczania poszczególnych elementów systemu jakości. W zakresie wykorzystania i stosowania materiałów odniesienia opisano nową metodę otrzymywania bez matrycowego materiału odniesienia lotnych analitów, opartą na wykorzystaniu procesu termicznego rozkładu związków powierzchniowych. Przedstawiono także wyniki uzyskane przez autora w trakcie 2-letniego stażu naukowego w IRMM dotyczące udziału w procesie produkcji certylikowanych materiałów odniesienia (badania certyfikacyjne, badania trwałości materiałów). Przedstawiono także wstępne prace związane z produkcją laboratoryjnego materiału odniesienia. W zakresie walidacji metod analitycznych opisano wyniki wieloletnich prac autora związanych z opracowywaniem i definiowaniem nowych procedur analitycznych. Przedstawiono charakterystykę metody oznaczania zawartości fluorków w próbkach ciekłych z wykorzystaniem elektrody jonoselektywnej. Zaprezentowano metodę wykorzystującą technikę chromatografii gazowej w badaniach kinetyki reakcji hydrolizy [Beta]-laktamów - efekt rocznego stażu naukowego w Universidad del Pais Vasco w San Sebastian, Hiszpania. Przedstawiono także wyniki badań walidacyjnych metody oznaczania zawartości etanolu w preparatach farmaceutycznych opartych na wy-korzystaniu techniki HS-GC-FID. Opracowana metoda została wdrożona do praktyki analitycznej w Zakładach Farmaceutycznych POLPHARMA SA w Starogardzie Gdańskim. W zakresie badań między laboratoryjnych przedstawiono wyniki udziału autora w badaniach organizowanych przez CCQM, w trakcie jego 2-letniego stażu w IRMM. Opisano także sposób przeprowadzania porównań między laboratoryjnych współorganizowanych przez autora i opracowywania ich wyników. Opisano, zaproponowany przez autora pracy, prosty, zrozumiały i przejrzysty sposób opracowywania wyników badań międzylaboratoryjnych. Przedstawiono współzależności między poszczególnymi elementami systemu jakości wyników pomiarów analitycznych. Końcowym efektem zainteresowań naukowych autora jest zaproponowany i opisany zintegrowany system kontroli jakości wyników pomiarów, w którego skład wchodzą: - jasno zdefiniowany sposób szacowania niepewności wyników pomiarów analitycznych, - wykorzystujące podstawy metrologii i elementy statystyki matematycznej, przejrzyste sposoby wyznaczania wartości poszczególnych parametrów walidacyjnych, - opracowany jasny i prosty tok postępowania przy opracowywaniu wyników porównań międzylaboratoryjnych, ułatwiający uczestnikom badań interpretację otrzymanych wyników, - przedstawienie reguł towarzyszących wykorzystywaniu materiałów odniesienia.

EN

The main problems connected with quality assessment, quality control and quality management of analytical measurements are presented in the thesis. Characteristics of QA/QC system elements, together with the current stale of traceability, uncertainty estimation, method validation, CRM application and participation in PT are described. The first part of this treatise presents basic definitions from the QA/QC system and methods of their calculations. In the second part, the author presents his contribution to the field of determination and the calculation of particular QA/QC parameters. Within the frame of reference material production and its application, a new method for preparation of a matrix-free reference material of volatile analytes, based on thermal decomposition of surface compounds, is described. The results of studies obtained during 2-year postdocs fellows at IRMM connected with the certification and stability of CRMs are presented. Preliminary research related to the production of laboratory reference material is described. Results of the author's works related to scientific description and definition of new analytical procedures in the field of method validation are presented. The potentiometric method of determination of fluoride content in liquid samples by ion selective electrode is described. Application of GC in the investigation of kinetic of hydrolysis reaction of [Beta]-lactams as a result of a one-year fellowship at Universidad del Pais Vasco in San Sebastian, Spain are presented. Results of calculations for validation parameters for the HS-GC-FID method used for determination of ethanol content in pharmaceuticals are presented as well. This method has been applied in analytical practice in the Pharmaceutical Factory POLPHARMA SA in Starogard Gdański, in Poland Within the framework of interlaboratory comparison, the results of a proficiency test organized by CCQM, in which the author participated during a 2-year fellowship at IRMM, are presented. Organization and elaboration of PTs results are described. A simple, clear and comprehensible system of PTs result elaboration, suggested by the author, is presented. Interrelations among particular QA/QC system components are presented. The final effect of the author's interest is suggested and described, integrated into a QA/QC system, which consist of: - a clearly defined method for estimation of uncertainty of analytical results, - transparent methods for the determination of validation parameters, based on metrology and statistics, - a clear and simple procedure used for the elaboration of PTs results, which helps their participants interpret obtained results, - a presentation of rules connected with CRM production and application.

Słowa kluczowe

PL

jakość pomiarów; walidacja metody; materiały odniesienia; badania międzylaboratoryjne; niepewność pomiaru

EN

quality of measurements; method validation; QA/QC system

• Wydawca: Wydawnictwo Politechniki Gdańskiej
• Czasopismo: Zeszyty Naukowe Politechniki Gdańskiej. Chemia
• Rocznik: 2007
• Tom: Nr 56(607)
• Strony: 3--67
• Opis fizyczny: Bibliogr. 140 poz., rys., tab.

Twórcy

autor

Konieczka P.

• Politechnika Gdańska, Katedra Chemii Analitycznej ul. Narutowicza 11/12

Bibliografia

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