Misiuk Wiesława
Institute of Chemistry, University of Białystok, 15-399 Białystok, Hurtowa 1, Poland.
Farmaco. 2005 Jan;60(1):61-9. doi: 10.1016/j.farmac.2004.09.004. Epub 2004 Dec 19.
Two simple, precise, and accurate extractive spectrophotometric methods have been developed for the determination of doxepin hydrochloride in pharmaceutical preparations. The methods are based on the formation of ion association complexes of doxepin with titanium (IV) and iron (III) thiocyanate complexes in acidic medium. The produced compounds are insoluble in water but well soluble in some organic solvents. They are extracted with mixtures of butyl alcohol-chloroform (2:3, v/v) and (1:4, v/v) and measured spectrophotometrically at 400 and 490 nm for DOX-Ti-SCN and DOX-Fe(III)-SCN methods, respectively. Beer's law was obeyed in the concentration ranges of 5-50 and 3-30 microg/ml with molar absorptivity of 7.12 x 10(3) and 1.36 x 10(4) l mol(-1) cm(-1) for DOX-Ti-SCN and DOX-Fe-SCN systems, respectively. The proposed methods have been successfully applied for the analysis of the drug in dosage forms. No interference was observed from common pharmaceutical adjuvants. The methods have been also used for the determination of the drug in the presence of its degradation product. Statistical comparison of the obtained results with the reference methods shows excellent agreement and indicates no significant difference in accuracy and precision.
已开发出两种简单、精确且准确的萃取分光光度法,用于测定药物制剂中的盐酸多塞平。这些方法基于在酸性介质中多塞平与钛(IV)和铁(III)硫氰酸盐络合物形成离子缔合络合物。生成的化合物不溶于水,但易溶于某些有机溶剂。用正丁醇 - 氯仿(2:3,v/v)和(1:4,v/v)的混合物萃取,对于DOX - Ti - SCN和DOX - Fe(III) - SCN方法,分别在400和490 nm处进行分光光度测定。DOX - Ti - SCN和DOX - Fe - SCN体系在5 - 50和3 - 30 μg/ml的浓度范围内符合比尔定律,摩尔吸光系数分别为7.12×10³和1.36×10⁴ l mol⁻¹ cm⁻¹。所提出的方法已成功应用于剂型中药物的分析。未观察到常见药物辅料的干扰。这些方法还用于在药物降解产物存在下测定药物。将所得结果与参考方法进行统计比较,结果显示出极好的一致性,表明在准确性和精密度方面无显著差异。