Determination of validation characteristics of the uv-spectrophotometric method of doxylamine quantitative determination in blood in the variant of the method of standard
Keywords:validation, bioanalytical methods, UV-spectrophotometry, doxylamine, method of standard
With the purpose of improvement of carrying out the quantitative determinations in forensic and toxicological analysis the possibility of application of the method of standard for UV-spectrophotometric determination of analytes in biological fluids has been studied. The procedure for determination and acceptability estimation of linearity, accuracy and precision for validation of such methods in the variant of the method of standard tested by the example of UV-spectrophotometric method of doxylamine quantitative determination in blood has been offered. The given procedure provides application of the normalized coordinates. For normalization of the experimental data obtained two approaches have been used: 1) Approach 1: the use of the reference solution with the concentration of the analyte corresponding to its concentration in the final spectrophotometric solution measured under the condition of zero losses for the point of 100% in the normalized coordinates. 2) Approach 2: the use of the reference sample with the concentration of doxylamine corresponding to its concentration for the point of 100% in the normalized coordinates. Estimation of linearity, accuracy and repeatability of the method at the first stage has been performed using the model solutions within the approach based on assumption of insignificance of the uncertainty of the analyte quantitative determination in model solutions in comparison with the complete uncertainty of the analysis results ΔAs. At the second stage determination of linearity, accuracy, repeatability and intermediate precision of the method has been carried out on the model samples prepared using the matrix for three parallel runs. It has been shown that the method of standard can be applied for UV-spectrophotometric determination of doxylamine in blood – Approach 1 is more acceptable.
Гризодуб А.И. Стандартизованные процедуры валидации методик контроля качества лекарственных средств. Аналитическая химия в создании, стандартизации и контроле качества лекарственных средств: В 3-х т. / Под ред. чл.-кор. НАН Украины В.П.Георгиевского. – Х.: НТМТ, 2011. – Т. 3. – 520 с.
Клименко Л.Ю., Трут С.Н., Петюнин Г.П., Иванчук И.М. // Укр. журн. клін. та лаборатор. медицини. – 2013. – Т. 8, №4. – С. 191-199.
Клименко Л.Ю. // Фармация Казахстана. – 2014. – №4. – С. 42-48.
Clarke’s analysis of drugs and poisons in pharmaceuticals, body fluids and postmortem material / Ed. by A.C.Moffat, M.D.Osselton, B.Widdop. – 4th ed. – London: Pharmaceutical Press, 2011. – 2609 p.
Guidance for Industry: Bioanalytical Method Validation / U.S. Department of Health and Human Services, Food and Drug Administration (FDA), Center for Drug Evolution and Research (CDER), Center for Veterinary Medicine (CVM). – Washington, DC: U.S. Government Printing Office, 2001. – 22 p.
Guidance for the Validation of Analytical Methodology and Calibration of Equipment used for Testing of Illicit Drugs in Seized Materials and Biological Specimens / United Nations Office on Drugs and Crime, Laboratory and Scientific Section. – New York: United Nations, 2009. – 70 p.
Guideline on Bioanalytical Method Validation / European Medicines Agency. Committee for Medicinal Products for Human Use (CHMP). – London, 2009. – 22 p.
Standard Practices for Method Validation in Forensic Toxicology (draft) / Scientific Working Group for Forensic Toxicology (SWGTOX). – 2012. – 52 p.
Copyright (c) 2014 National University of Pharmacy
This work is licensed under a Creative Commons Attribution 4.0 International License.Authors who publish with this journal agree to the following terms:
- Authors retain copyright and grant the journal right of first publication with the work simultaneously licensed under a Creative Commons Attribution License that allows others to share the work with an acknowledgement of the work's authorship and initial publication in this journal.
- Authors are able to enter into separate, additional contractual arrangements for the non-exclusive distribution of the journal's published version of the work (e.g., post it to an institutional repository or publish it in a book), with an acknowledgement of its initial publication in this journal.
- Authors are permitted and encouraged to post their work online (e.g., in institutional repositories or on their website) prior to and during the submission process, as it can lead to productive exchanges, as well as earlier and greater citation of published work (See The Effect of Open Access).