蒙脱石及其制剂吸附力测定方法研究

目的：对现行蒙脱石及其制剂质量标准中吸附力检查的原理及方法进行深入研究，拟以非毒性试剂三氯六氨合钴（Ⅲ）替代目前所使用的价格昂贵且剧毒的硫酸士的宁测定蒙脱石吸附力。方法：经对蒙脱石吸附力测定原理的理论论证，优化了吸附力测定方法，利用正交设计软件确定反应条件为37℃水浴放置1 h，以紫外-可见分光光度法在474 nm测定，对方法的线性、精密度和溶液稳定性进行了方法学验证。结果：经对21家企业的39批原料与制剂样品测定，原料结果在1.024~1.174 mmol·g^-1之间，散剂结果在1.018~1.238 mmol·g^-1之间，分散片结果在0.894~1.130 mmol·g^-1之间，所有样品结果与采用硫酸士的宁测定吸附力的结果间换算平均系数为0.43，与理论推导一致，方法可行。结论：三氯六氨合钴（Ⅲ）可替代硫酸士的宁作为蒙脱石吸附力测定的标志物，试验安全，无污染，经济，简便。

Objective: To study the theory and method of adsorption capacity examination of the quality standard for montmorillonite and its preparation. The montmorillonite adsorption measurement of nontoxic reagent hexaamminecobalt(Ⅲ)cholride instead of expensive and toxic strychninesulfate were investigated.Methods: Based on the demonstration principle of bymontmorillonite adsorption, the method of adsorption determination of montorillonite was optimized. The parameters including the temperature, the vibration wave velocity and time and the reaction conditions were used for the orthogonal experimental design. Water bath was 37℃ for 1 h and the UVvisible spectrophotometry wavelength was 474 nm. The method of linearity, precision and stability were validated.Results: The 39 batches of raw materials and preparations from 21 companies were determined. The content range of the raw material was 1.024-1.174 mmol·g^-1 and the content range of the powder was 1.018~1.238 mmol·g^-1. The content range of the dispersible tablets was 0.894-1.130 mmol·g^-1. The conversion average coefficient of all the results determined by hexaamminecobalt(Ⅲ)cholride was 0.43 compared with strychninesulfate adsorption method, which is consistent with the theory, the method is feasible.Conclusion: Hexaamminecobalt (Ⅲ)cholride can be used for measuring the adsorption of montmorillonite and this method is test-safe, pollutionfree, economic and convenient.

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