用MBTH和铁氰化钾氧化偶联法测定剂量型儿茶酚胺

S. Ashour
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引用次数: 2

摘要

建立了一种新的直接比色法测定纯制剂和制剂中儿茶酚胺(甲基多巴,MD)含量。该方法是将MD与3-甲基-2-苯并噻唑啉酮肼盐酸盐一水合物(MBTH)和铁氰化钾在pH为10.4的水溶液中氧化偶联反应,生成最大吸收波长为460 nm的橙色产物。比尔定律图在1.0 ~ 56.0µg mL-1的浓度范围内相关性良好,检出限为0.31µg mL-1。该方法的摩尔吸光度为6.56×103 L mol-1 cm-1。所有测量均在25±1.0℃下进行,有色物质的形成常数(logKf)值为9.48,标准自由能(DG‡)为−54.09 KJ mol-1。该方法成功地应用于片剂中MD的测定,并与USP法进行了比较。在片剂中用作添加剂的常见赋形剂不干扰所建议的方法。该方法准确、精密度高,重现性好,操作简单、成本低、耗时短,适用于原料药和剂型MD的常规分析。
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A novel sensitive colorimetric determination of catecholamine drug in dosage form via oxidative coupling reaction with MBTH and potassium ferricyanide
A new and direct colorimetric method has been established for the determination of catecholamine (methyldopa, MD) in both pure form and in pharmaceutical formulations. The method is based on the oxidative coupling reaction of MD with 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) and potassium ferricyanide at pH 10.4 in aqueous medium to form an orange product that has a maximum absorption at 460 nm. Beer's law plot showed good correlation in the concentration range of 1.0−56.0 µg mL-1, with detection limit of 0.31 µg mL-1. Molar absorptivity for the above method was found to be 6.56×103 L mol-1 cm-1. All the measurements were carried out at 25 ± 1.0 °C, the formation constant (logKf) value of colored species is 9.48 and the standard free energy (DG‡) is − 54.09 KJ mol-1. This method was applied successfully to determination of MD in tablets and the results were compared with the USP method. Common excipients used as additives in tablets do not interfere in the proposed method. The method is accurate, precise and highly reproducible, while being simple, cheap and less time consuming and hence can be suitably applied for routine analysis of MD in bulk and dosage forms.
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