259 resultados para Flow rate variation
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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An accurate, sensitive, precise and rapid reversed-phase high-performance liquid chromatographic method was successfully developed and validated for the determination of caffeic acid (CA) in emulsions. The best separation was achieved on a 250 × 4.6 mm, 5.0 µm particle size RP18 XDB Waters column using ethanol and purified water (40:60 v/v) adjusted to pH 2.5 with acetic acid as the mobile phase at a flow rate of 0.7 mL/min. Ultraviolet detection was performed at 325 nm at ambient column temperature (25°C). The method was linear over the concentration range of 10-60 µg/mL (r(2) = 0.9999) with limits of detection and quantification of 1.44 and 4.38 µg/mL, respectively. CA was subjected to oxidation, acid, base and neutral degradation, as well as photolysis and heat as stress conditions. There were no interfering peaks at or near the retention time of CA. The method was applied to the determination of CA in standard and pharmaceutical products with excellent recoveries. The method is applicable in the quality control of CA.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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A stability-indication high performance liquid chromatographic method has been developed for the determination of norfloxacin in tablet dosage forms. Optimum separation was achieved in less than 7 minutes using Eclipse Plus Zorbax C18 Agilent, 150 mm×4.6 mm i.d., 5 μm particle size column. The analyte was resolved by using a mobile phase 5% acetic acid aqueous solution and methanol (80:20, v/v) at a flow rate 1.0 ml/min on an isocratic high performance liquid chromatographic system at a wavelength of 277 nm. Linearity, system suitability, precision, sensitivity, selectivity, specific, and robustness were established by International Conference Harmonization guidelines. For stress studies the drug was subjected to photolysis, oxidation, acid, alkaline and neutral conditions. The analytical conditions and the solvent developed provided good resolution within a short analysis time and economic advantages. The proposed method not required sophisticated and expensive instrumentation.
Validation of analytical methodology for quantification of cefazolin sodium by liquid chromatography
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A reversed-phase high performance liquid chromatography method was validated for the determination of cefazolin sodium in lyophilized powder for solution for injection to be applied for quality control in pharmaceutical industry. The liquid chromatography method was conducted on a Zorbax Eclipse Plus C18 column (250 x 4.6 mm, 5 μm), maintained at room temperature. The mobile phase consisted of purified water: acetonitrile (60: 40 v/v), adjusted to pH 8 with triethylamine. The flow rate was of 0.5 mL min-1 and effluents were monitored at 270 nm. The retention time for cefazolin sodium was 3.6 min. The method proved to be linear (r2 =0.9999) over the concentration range of 30-80 µg mL-1. The selectivity of the method was proven through degradation studies. The method demonstrated satisfactory results for precision, accuracy, limits of detection and quantitation. The robustness of this method was evaluated using the Plackett–Burman fractional factorial experimental design with a matrix of 15 experiments and the statistical treatment proposed by Youden and Steiner. Finally, the proposed method could be also an advantageous option for the analysis of cefazolin sodium, contributing to improve the quality control and to assure the therapeutic efficacy
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Pós-graduação em Agronomia (Irrigação e Drenagem) - FCA
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)