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1.
Journal of Huazhong University of Science and Technology (Medical Sciences) ; (6): 752-757, 2016.
Artículo en Inglés | WPRIM | ID: wpr-238451

RESUMEN

This study aimed to conduct measurement uncertainty assessment of a new method for determination of Sudan colorants (Sudan I, II, III and IV) in food by high performance liquid chromatography (HPLC). Samples were extracted with organic solvents (hexane, 20% acetone) and first purified by magnesium trisilicate (2MgO·3SiO2). The Sudan colorants (Sudan I-IV) were also initially separated on C8 by gradient elution using acetonitrile and 0.1% (v/v) formic acid aqueous solution as the mobile phases and detected with diode-array detector (DAD). The uncertainty of mathematical model of Sudan I, II, III and IV is based on EURACHEM guidelines. The sources and components of uncertainty were calculated. The experiment gave a good linear relationship over the concentration from 0.4 to 4.0 μg/mL and spiked recoveries were from 74.0% to 97.5%. The limits of determination (LOD) were 48, 61, 36, 58 μg/kg for the four analytes, respectively. The total uncertainty of Sudan colorants (Sudan I, II, III and IV) was 810±30.8, 790±28.4, 750±27.0, 730±50.0 μg/kg, respectively. The recovery uncertainty was the most significant factor contributing to the total uncertainty. The developed method is simple, rapid, and highly sensitive. It can be used for the determination of trace Sudan dyes in food samples. The sources of uncertainty have been identified and uncertainty components have been simplified and considered.


Asunto(s)
Humanos , Compuestos Azo , Química , Cromatografía Líquida de Alta Presión , Métodos , Análisis de los Alimentos , Métodos , Colorantes de Alimentos , Química , Límite de Detección , Silicatos de Magnesio , Química , Naftoles , Química
2.
Artículo en Inglés | IMSEAR | ID: sea-168517

RESUMEN

A new high performance liquid chromatography (HPLC) with ultraviolet detection method is developed for the simultaneous quantification of acetaminophen and tramadol in bulk and in its combined pharmaceutical dosage form. The chromatographic separation was performed on Waters symmetry C8 column (250 mm × 4.6 mm I.D., 5 μm particle size) using isocratic elution. The optimized mobile phase consists of phosphate buffer (pH 6.8) and methanol (80:20, v/v). The eluted analytes are monitored at 215 nm wavelength using a UV detector. The developed method separates acetaminophen and tramadol within a run time of 6 min. The developed method was validated as per International Conference of Harmonization guidelines with respect to linearity, sensitivity (limit of detection and limit of quantification), selectivity, accuracy, precision and robustness. The developed and validated method was successfully applied to the determination of acetaminophen and tramadol in combined pharmaceutical dosage forms without any interference from the excipients with good recovery, precision and accuracy.

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