基于低场核磁共振技术仙草方泡腾片颗粒含水量及水分相态分布研究

Determination of water content and moisture distribution of Xiancao Prescription effervescent granules by low field nuclear magnetic resonance imaging

目的应用快速、准确、无损的低场核磁共振技术,测定仙草方泡腾片颗粒的含水量及水分相态分布。方法通过标定4个不同质量的Mn Cl2溶液的频率鉴别信号(FID)幅值,拟合出水分量与FID信号幅值的标准曲线方程,再选取干、湿法制粒所得泡腾片颗粒各3份,分别测定其FID幅值,根据拟合标准曲线方程计算干、湿法颗粒含水量,同时将低场核磁共振技术测得的含水量结果与药典收录的减压干燥法进行比较分析。结果低场核磁共振测定仙草方泡腾片颗粒的含水量方便快速,结果稳定准确,通过与减压干燥法对比发现,核磁共振法比减压干燥法测得的含水量高的值不超过0.3%。结论减压干燥法无法将仙草方泡腾片颗粒内部的结合水完全干燥,而核磁共振法测得的是泡腾片颗粒内部结合水、束缚水和自由水的总和,且能清晰展示颗粒中3种不同相态水分子的分布及运动性能,为药品制造过程中物性参数的研究提供了一种有效方法。

Objective To determine the water content and water phase distribution of Xiancao prescription effervescent granules by a more rapid, accurate and non-destructive low-field NMR instrument. Methods The standard curve equation of water content and FID signal amplitude was fitted by calibrating the FID signal amplitude of four different mass of manganese chloride solutions. Three parts of Xiancao prescription effervescent granules were obtained by dry and wet granulation to test their FID signals and calculated the water content of dry and wet granulation by the fitting standard curve equation; Then the results were compared according to decompression drying of pharmacopeia standard. Results The water content of effervescent tablets was convenient and rapid, and the result was stable and accurate. Compared with the standard decompression drying method, the water content measured by low field NMR instrument was less than 0.3%. Conclusion Due to the decompression drying method can＇t be Xiancao prescription effervescent granules within the bound water completely dry, sum of effervescent granules particles inside bound water and free water instrument is measured by low-field NMR, which can clearly show an effective method for the study of physical properties of three different phase water molecules in the process of drug manufacturing.