Cadena Pabyton G, Oliveira Eric C, Araújo Alberto N, Montenegro Maria C B S M, Pimentel Maria C B, Lima Filho José L, Silva Valdinete L
Laboratório de Imunopatologia Keizo Asami (LIKA), Universidade Federal de Pernambuco (UFPE), Av. Prof. Moraes Rego, s/n, 50780-901, Recife, Pernambuco, Brazil.
Lipids. 2009 Nov;44(11):1063-70. doi: 10.1007/s11745-009-3353-z. Epub 2009 Oct 11.
An expeditious colorimetric methodology for the determination of the deoxycholic acid (DCA) and of the ursodeoxycholic acid (UDCA) in pharmaceutical formulations is reported. The method is based on their competitive complexation reaction with a color indicator to form beta-cyclodextrin-inclusion complexes. Several pH color indicators were tested, but phenolphthalein (PHP) showed the best interaction with the beta-cyclodextrin (beta-CD) with an inclusion yield higher than 95%. The best concentrations of beta-cyclodextrin to form inclusion complexes were 1.24 x 10(-3) and 6.2 x 10(-4) M at pH 9.5 and 10.5. Statistical analysis of the results showed that the pH had a significant effect on the DCA determination and that high beta-CD-PHP inclusion complex concentrations had a significant negative effect on the UDCA determination (p < 0.05). The limit of detection and limit of quantification were 3.94 x 10(-5) and 1.31 x 10(-4) M for DCA (range: 6.1 x 10(-6)-3.13 x 10(-3) M), 4.08 x 10(-5) and 1.36 x 10(-4) M for UDCA (range: 6.05 x 10(-6)-3.88 x 10(-4) M). This simple and cheap method showed high stability and feasible instrumentation.
本文报道了一种快速比色法,用于测定药物制剂中的脱氧胆酸(DCA)和熊去氧胆酸(UDCA)。该方法基于它们与一种颜色指示剂的竞争性络合反应,形成β-环糊精包合物。测试了几种pH颜色指示剂,但酚酞(PHP)与β-环糊精(β-CD)的相互作用最佳,包合产率高于95%。在pH 9.5和10.5时,形成包合物的最佳β-环糊精浓度分别为1.24×10⁻³和6.2×10⁻⁴ M。结果的统计分析表明,pH对DCA测定有显著影响,高浓度的β-CD-PHP包合物对UDCA测定有显著负面影响(p < 0.05)。DCA的检测限和定量限分别为3.94×10⁻⁵和1.31×10⁻⁴ M(范围:6.1×10⁻⁶ - 3.13×10⁻³ M),UDCA的检测限和定量限分别为4.08×10⁻⁵和1.36×10⁻⁴ M(范围:6.05×10⁻⁶ - 3.88×10⁻⁴ M)。这种简单且廉价的方法具有高稳定性和可行的仪器设备。