Results convergence of pharmacopoeial tests by titrimetric methods: acceptance criteria and experimental parameter
DOI:
https://doi.org/10.15587/2519-4852.2016.76358Keywords:
quality assurance, pharmacopoeial test, volumetric titration, uncertainty, convergencey, acceptance criteriaAbstract
Quality assurance of test results is one of the topical issues of analytical laboratories functioning. Scientifically reasonable criteria and recommendations in relation to the scheme and quality control of pharmacopoeial tests results by volumetric titration methods were developed by the authors according to the previous studies results. The criteria were elaborated by results of test uncertainty estimation.
Aim of research was experimental verification of the requirements to results repeatability of pharmacopoeial tests by titrimetric methods developed on the basis of the scientific reasoning.
Methods. Authors used the statistical analysis methods of chemical experiment results.
Results. Experimental data of the test results by titrimetric methods, obtained in a separate laboratory and in an interlaboratory experiment, were examined. The displayed results belong to the most wide spread pharmacopoeial titration methods for substances: titration with the perchloric acid solution in acetic acid with the visual fixing of end point; potentiometric titration with perchloric acid solution in acetic acid, potentiometric titration of halogen salts of organic bases by the difference of volumes between two potential leaps; aqueous titration with the visual fixing of end point; potentiometric titration with aqueous titrant. Requirements to convergence, elaborated by results of the uncertainty test estimation of titrimetric methods, meet the examined data main parameters. Relevant amount of simultaneous tests, that will be sufficient for the achievement of the recommended values for relative standard deviation of the mean folds, is middle from three to four.
Conclusion. The acceptability criteria developed on scientific reasoning basis meet the main parameter of titrimetric methods tests and can be recommended for the use in- functioning of pharmaceutical analytical laboratoriesReferences
- Zagal'ni vymogy do kompetentnosti vyprobuval'nyh ta kalibruval'nyh laboratorij (ISO/IEC 17025:2005, IDT): DSTU ISO/IEC 17025:2006 (2007). Kyiv: Derzhspozhyvstandart Ukrai'ny, 33.
- Leont'ev, D. A., Grizodub, A. I. (2007). Metrologicheskij kontrol' kachestva rezul'tatov izmerenij. Farmakom, 2, 16–25.
- Georgievskij, V. P.; Georgievskij, V. P. (Ed.) (2011). Kislotno-osnovnoe titrovanie v nevodnyh sredah. Vol. 1. Analiticheskaja himija v sozdanii, standartizacii i kontrole kachestva leakrstvennyh sredstv. Kharkov: izd. NTMT, 12–95.
- Sur, S. V., Kovalenko, S. M., Gubar', S. M. et. al. (2013). Algorytm zagal'nogo ocinjuvannja krytychnyh faktoriv na pidstavi upravlinnja ryzykamy dlja jakosti rezul'tativ vyprobuvan' metodom tytrymetrii'. Informacijnyj lyst pro novovvedennja v sferi ohorony zdorov’ja. Kyiv: Ukrmedpatentinform MOZ Ukrai'ny, 8.
- 4.2. Volumetric analysis (2013). European Pharmacopoeia. Strasbourg: European Directorate for the Quality of Medicines, Council of Europe, 545–550.
- Chikalova, S. O., Grizodub, A. I. (2011). Ocenka neopredelennosti metodik titrovanija substancij s ispol'zovaniem poshagovogo pohoda. Farmakom, 3, 11–31.
- Chikalova, S. O., Grizodub, A. I. (2012). Kriterii priemlemosti rezul'tatov kontrolja kachestva substancij pri ispol'zovanii metoda titrovanija. Farmakom, 3, 41–54.
- Sur, S. V., Gryzodub, O. I., Gubar', S. M. et. al. (2009). Rezul'taty kil'kisnogo vyznachennja testovogo zrazka substancii' natriju acetatu trygidratu laboratorijamy z kontrolju jakosti likars'kyh zasobiv u 6-mu raundi programy profesijnogo testuvannja laboratorij. Farmakom, 4, 11–19.
- Daas, A. G. J., Miller, J. H. M. (1998). Content limits in the European Pharmacopoeia (Part 2). Pharmeuropa, 10 (1), 137–146.
- Statystychnyj analiz rezul'tativ himichnogo eksperymentu. Derzhavna Farmakopeja Ukrai'ny. Vol. 1 (2015). Kharkiv: Derzhavne pidpryjemstvo “Naukovo-ekspertnyj farmakopejnyj centr”, 881–909.
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Copyright (c) 2016 Світлана Олегівна Чикалова, Олександр Іванович Гризодуб, Олена Валеріївна Бевз, Ірина Григорівна Зинов'єва, Галина Вікторівна Кобець
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