University of Khartoum, Faculty of Pharmacy, P.O. Box 1996, Khartoum, Sudan.
Saudi Pharm J. 2009 Oct;17(4):289-93. doi: 10.1016/j.jsps.2009.10.005. Epub 2009 Nov 10.
A new, simple and low cost spectrophotometric method for the determination of methyldopa in pharmaceutical preparations was developed. The method was based on the coupling of methyldopa with 2,6-dichloroquinone-4-chlorimide (DCQ). The absorbance maximum (λ max) of the resulted colored product was at 400 nm. Different buffers were used to determine the optimal pH for the reaction. About 1% w/v acetate buffer with pH 8.0 gave the optimal pH required for the reaction. Of the different solvents tried, water and ethanol were found to be the most suitable solvents. Beer's law was obeyed in concentration range of 4-20 μg/ml methyldopa. The correlation coefficient was found to be (r = 0.9975). The limit of detection and limit of quantification were 1.1 μg/ml and 3.21 μg/ml, respectively. The reaction ratio between methyldopa and DCQ was studied and found to be 1:3. The work included the study of the possible interference of hydrochlorothiazide found in combination with methyldopa tablets. The method was validated and results obtained for the assay of two different brands of methyldopa tablets were compared with the BP method (colorimetric). The repeatability and reproducibility of the developed method were evaluated and the obtained results quoted. The derivative formed as a result of the reaction of methyldopa with DCQ was isolated and its possible mechanistic pathway was suggested.
一种新的、简单且低成本的分光光度法用于测定药物制剂中的甲基多巴。该方法基于甲基多巴与 2,6-二氯-4-氯亚胺(DCQ)的偶联。所得有色产物的最大吸收波长(λmax)在 400nm 处。使用不同的缓冲液来确定反应的最佳 pH 值。约 1%w/v 的乙酸盐缓冲液(pH 8.0)提供了反应所需的最佳 pH 值。在所尝试的不同溶剂中,发现水和乙醇是最合适的溶剂。在 4-20μg/ml 甲基多巴浓度范围内,比尔定律得到了遵守。相关系数为(r=0.9975)。检测限和定量限分别为 1.1μg/ml 和 3.21μg/ml。研究了甲基多巴与 DCQ 的反应比例,发现为 1:3。研究了与甲基多巴片剂联合使用的氢氯噻嗪可能产生的干扰。该方法已得到验证,并将两种不同品牌的甲基多巴片剂的测定结果与 BP 方法(比色法)进行了比较。评估了所开发方法的重复性和重现性,并引用了获得的结果。还分离了甲基多巴与 DCQ 反应形成的导数,并提出了其可能的反应途径。