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Simple, fast, and sensitive isocratic high-performance liquid chromatography method for the quantification of latanoprost

Mansoor S., Tas C.

Acta Chromatographica

2014

Vol. 26, no. 2

191--202

A simple, sensitive, fast, and accurate isocratic high-performance liquid chromatography (HPLC) method with UV detection (205 nm) has been developed and validated for the quantification of latanoprost (in nanogram level) in pure and commercial dosage form. An Agilent Eclipse XDB-C18 column (150 × 4.6 mm i.d., 3.5 μm particle size) was used. Chromatography was performed with a mobile phase containing a mixture of acetonitrile and water (70:30, v/v) containing 0.1% v/v trifluoroacetic acid, adjusted at pH 3.0 at a flow rate of 1 mL min-1. Each analysis required 3.0 min including triamcinolone acetonide as an internal standard. The method was validated for linearity, accuracy, precision, specificity, system suitability, and robustness. The calibration curve was linear in the concentration range 0.0125–1 μg mL-1; the correlation coefficient was 0.999. The method proved to be accurate, precise, specific, rapid, and reproducible according to ICH standards. The method showed good recoveries (average 100.15 %), and the relative standard deviations of intra- and inter-day were <2.0%. This method is novel since there has been no report about analysis of latanoprost at ng mL-1 levels using a simple HPLC method. Besides regular quality control assay of latanoprost in raw material and in commercial formulations, this method has key importance for scientists working on sustained drug delivery system of latanoprost in which quantification in nanogram levels is one of the most important parameters.

Determination of triamcinolone acetonide in pharmaceutical formulation and human serum by adsorptive cathodic stripping voltammetry

Hammam E.

Chemia Analityczna

2007

Vol. 52, No. 1

43-53

Electrochemical behavior of triamcinolone acetonide (TAA) has been studied by cyclic voltammetry at a hanging mercury drop electrode in universal buffers of pH 2-11. Due to the interfacial adsorption of triamcinolone acetonide onto the mercury surface, a fully validated square-wave adsorptive cathodic stripping voltammctric procedure was developed for its determination in the bulk form. Under optimized conditions, the stripping voltammetric peak current of triamcinolone acetonide showed a linear dependence on TAA concentration over the range 1 x 10-9-9 x 108 mol L-1. The mean percentage recovery of TAA was 99.84 š 0.64, the detection limit {LOD) was 3 x 10-10 mol L-1, and the quanlitation limit (LOQ) equaled 1 x 10-9 mol L-1. The proposed procedure was successfully applied in the determination of triamcinolone acetonide in Kenacort'K tablets and in human serum spiked with TAA without any pretreatment and/or time-consuming extractions prior to the analysis. LOD and LOQ corresponding to the determination of triamcinolone acetonide in spiked human serum were 7.5 x10-10 mol L-1 and 2,5 x 10-9mol L-1, respectively.

Badano elektrochmiczne zachowanie acetonidu triamcinolonu (TAA) metodą cyklicznej woltamperometrii na elektrodzie rtęciowej w przedziale pH 2-11. Ponieważ stwierdzono adsorpcję TAA na powierzchni rtęci, do oznaczania tego związku zastosowano procedurę wykorzystującą wiszącą elektrodę rtęciową i adsorpcyjną, katodową woltamperometrię strippingową, W warunkach optymalnych otrzymano liniową zależność między wysokością piku woltamperometrycznego i stężeniem TAA w zakresie 1 x 10-9-9x 10-8mol L-1. Średni odzysk wyniósł 99.84 š 0.64 %, granica wykrywalności 3 x 10-9 mol L-1 a granica oznaczalności l x 10-9 mol L-1. Opacowaną procedurę zastosowano do oznac/.ania TAA w tabletkach Kenacort* i w ludzkiej surowicy krwi po dodaniu analitu. Nie było porzeby przeprowadzenia wstępnych działań chemicznych i ekstrakcji. Granicę wykrywalności i granicę oznaczalności w surowicy krwi oznaczono odpowiednio jako 7,5 x 10-10 mol L-1 i 2,5x 10 mol L-1.