pharmaceutical analysis
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241 s.
In the last few years, there has been a resurgence of supercritical fluid chromatography (SFC), which has been stimulated by the introduction of a new generation of instruments and columns from the main providers of chromatographic instrumentation, that are strongly committed to advancing the technology. The known limitations of SFC, such as weak UV sensitivity, limited reliability and poor quantitative performance have been mostly tackled with these advanced instruments. In addition, due to the obvious benefits of SFC in terms of kinetic performance and its complementarity to LC, advanced packed-column SFC represents today an additional strategy in the toolbox of the analytical scientist, which may be particularly interesting in pharmaceutical analysis. In the present review, the instrumentation and experimental conditions (i.e. stationary phase chemistry and dimensions, mobile phase nature, pressure and temperature) to perform "advanced SFC" are discussed. The applicability of SFC in pharmaceutical analysis, including the determination of drugs in formulations and biofluids is critically discussed.
sv.
- MeSH
- farmaceutická chemie MeSH
- léčivé přípravky analýza MeSH
- Publikační typ
- periodika MeSH
- Konspekt
- Farmacie. Farmakologie
- NLK Obory
- farmacie a farmakologie
- farmacie a farmakologie
- biochemie
Rádionuklidová rontgenofluorescenčná analýza (RRFA) sa používa na identifikáciu a stanovenie prvkov s Z>18. Vo farmácii sa ňou môžu stanoviť obsahy prvkov v liečivách a farmaceutických pomocných látkach. Metóda umožňuje rozlíšenie ťažkých kovov pri skúškach na čistotu liečiva. Zároveň je ňou možné overovať pôvod suroviny alebo liečiva na základe jeho prvkového zloženia. Práca sa zaoberá prípravou vzoriek farmaceutických pomocných látok na stanovenie obsahu prvkov Fe, Cu, Zn, Pb metódou RRFA s použitím rádionuklidového zdroja 238Pu. Na stanovenie obsahu prvkov boli pripravené 3 druhy štandardov s cieíom odstránenia vplyvu absorpčných vlastností vzorky. Výsledky so štatistickým zhodnotením presnosti merania sú uvedené v tabuľkách. V práci bola prevedená analýza 7 vzoriek plnív, 3 vzoriek želatíny, 2 vzoriek SILOXID-u, 1 vzorky AEROSIL-u.
X-ray fluorescence analysis (XRF) has been employed for the identification and determination of elements with Z>18. In pharmacy, it can be used to determine the content of elements in drugs and pharmaceutical auxiliary substances. The method makes it possible to distinguish heavy metals in the tests of purity of drugs. It can also be used to verify the origin of the raw material or drug on the basis of its elemental composition. The present paper is concerned with the preparation of samples of pharmaceutical auxiliary substances for the determination of the content of the elements Fe, Cu, Zn, and Pb by the XRF method with the use of a radionuclide source of 238Pu. For the determination of the content of elements, three kinds of standards were prepared aiming to remove the effect of absorption properties of the sample. The results with statistical evaluations of precision of measurement are tabulated. The study carried out an analysis of 7 samples of fillers, 3 samples of gelatine, 2 samples of SILOXID, and 1 sample of AEROSIL.
Thermal analysis is a valuable method in pharmaceutical research. A wide range of thermal methods are used in drug development like thermogravimetry (TG), diffe¬rential thermal analysis (DTA), differential scanning calori¬metry (DSC) and other sensitive and specific methods. The present review deals with application of these me¬thods in characterization of drugs and excipients, such as their polymorph stability, glass transition temperature, purity analysis and compatibility of drugs.
- Klíčová slova
- termické metody, farmaceutický vývoj, DSC, skelný přechod, polymorfismus, kompatibilita,
- MeSH
- chemické techniky analytické MeSH
- diferenciální skenovací kalorimetrie metody MeSH
- farmaceutická technologie MeSH
- fyzikální chemie MeSH
- léčivé přípravky MeSH
- příprava léků MeSH
- termografie metody MeSH
- termogravimetrie metody MeSH
- výzkum MeSH
- Publikační typ
- práce podpořená grantem MeSH
... Form Selection of Pharmaceutical Compounds 1 -- Ann W. Newman and G. Patrick Stáhly -- 2. ... ... Preparation of Drug Samples for Analysis 59 -- David E. Nadig -- 3. ... ... Mass Spectroscopy in Pharmaceutical Analysis 151 -- Frank J. Belas and Ian A. Blair -- 5. ... ... Applications of Capillary Electrophoresis Technology in the -- Pharmaceutical Industry 313 -- Charles ... ... Statistical Considerations in Pharmaceutical Process -- Development and Validation 537 -- Gerald J. ...
- Klíčová slova
- Příručky, Farmaceutická analýza, analýza léčiv,
- Publikační typ
- příručky MeSH
- Konspekt
- Fyzioterapie. Psychoterapie. Alternativní lékařství
- NLK Obory
- farmacie a farmakologie
The ultra-performance liquid chromatography (UPLC) method, which involves pre-column derivatization of nitrite with 2,3-diaminonaphthalene (DAN) to form 2,3-naphthotriazole (NAT), offers the advantages of easy sample preparation, simple derivatization, stable derivatives, rapid analysis, high sensitivity and specificity and lack of interferences for determining nitrite in pharmaceutical samples. Determination of NAT was performed on a an Acquity UPLC HSS T3 column using a gradient elution of 0.1% formic acid with acetonitrile at flow rate of 0.4 mL/min and temperature at 45 °C. The single-quadrupole mass detector was operated in the positive ion mode. Quadrupole mass analyser was employed in selected ion monitoring mode using a target ion at m/z = 170 as [M+H]+. The UPLC-MS method was validated as per International Council on Harmonization (ICH) guidelines in terms of linearity, limit of detection, limit of quantification, selectivity, accuracy, precision, intermediate precision and stability. The UPLC-MS method was demonstrated to be applicable for the determination of nitrite in various pharmaceutical samples. The proposed UPLC-MS method was used to study the effect of nitrite content in pharmaceutical products on the formation of N-nitrosamines. The high importance of nitrites in relation to the N-nitrosation reaction was discussed. As deduced from theory and justified by the presented results, reducing the nitrite concentration could definitely solve the N-nitrosamine contamination. Nitrites, unlike secondary and tertiary amines, are universal precursors to any N-nitrosamine, so this solution is easily transferable to any relevant pharmaceutical product.
