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Determination of fluoxetine in the presence of photodegradation products appearing during UVA irradiation in a solid phase by chromatographic-densitometric method, kinetics and identification of photoproducts

Maślanka A., Hubicka U., Krzek J., Walczak M., Izworski G.

Acta Chromatographica

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2013

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Vol. 25, no. 3

465--481

EN

An effect of ultraviolet A (UVA) radiation on fluoxetine stability in solid phase with and without the presence of selected metal ions was studied using the chromatographic-densitometric method. Silica gel TLC F254 plates were used as the stationary phase and chloroform-methanol-ammonia 25% (45:4.5:0.5, v/v/v) as the mobile phase. The chromatograms were recorded densitometrically at a wavelength of λ = 260 nm.Both the concentration and kind of an ion have an effect on the photodegradation process. Kinetic studies demonstrated that fluoxetine photodegradation is the fastest in the presence of Cu(II) ions, decreases in the presence of Fe(III) and Fe(II) ions, and is the lowest in the presence of Al(III) ions. Under conditions established without the presence of metal ions, fluoxetine maintains photostability.The liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI/MS) method was applied for the identification of decomposition products noting the presence of 3-phenyl-3-hydroxypropylamine and 4-trifluoromethylphenol.

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Evaluation of a CGC-FID method for qualitative and quantitative analysis of azole antifungal drugs

Ekiert R. J., Krzek J., Czekaj J. S., Hubicka U.

Acta Chromatographica

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2009

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Vol. 21, no. 2

273--282

EN

This paper presents a new method for identification and quantitative analysis of six azole antifungal drugs — bifonazole, clotrimazole, econazole, fluconazole, ketoconazole, and miconazole — by capillary gas chromatography (CGC) combined with flame ionization detection (FID). The chromatographic separation conditions were established and the method was validated for precision (RSD = 1.49–3.55%), recovery (98.6–101.2%), and linearity within the range under investigation (∼1.0–33.3 ng). The results obtained show the newly developed procedure is suitable for qualitative and quantitative pharmaceutical analysis of the six azoles.

3

Qualitative and quantitative analysis of hesperidin in tablets by thin layer chromatography with densitometric UV detection

Janeczko Z., Hubicka U., Podolak I., Krzek J.

Chemia Analityczna

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2004

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Vol. 49, No. 3

309-316

EN

Conditions for detection of hesperidin in pharmaceutical formulations, such as Hesperydynin tablets, have been established. Chromatographic separation was performed on 60 F254 silica gel TLC plates with a chloroform-methanol-water (23+12+2, v/v/v) mobile phase. The spots were analysed by UV densitometry at [lambda] ≈ 286 nm. Under the established experimental conditions repeatable and accurate results were obtained. The method proposed is sensitive. It provides detection limit of 20 ng and satisfactory recovery in the range: 99.91%-100.74% for the declared content 100 mg. Linearity was maintained in the broad range from 4 to 44 žg mL-1.

PL

Opracowano warunki identyfikacji hesperydyny w preparatach farmaceutycznych na przykładzie tabletek Hesperydynin. Rozdział chromatograficzny przeprowadzono na pfytkach TLC pokrytych żelem krzemionkowym 60 F(254), z fazą ruchomą o składzie chloroform -metanol woda (23+12+2 v/v/v). Zastosowano detekcję densytometryczną UV przy długości fali Lambda = 286 nm. W zastosowanych warunkach uzyskano dokładne i powtarzalne wyniki oznaczeń. Czułość metody jest wysoka, granica wykrywalności wynosi 20 ng. Odzysk hesperydyny z próbki o deklarowanej zawartości związku 100 mg wahał się w granicach 99.91%-100.74%. Stwierdzono szeroki zakres Siniowości: od 4 do 44 ug mL(-1).