玉竹多糖铁配合物的制备工艺优化及铁含量测定

目的: 优化选择玉竹多糖铁配合物的合成工艺并确立测定铁含量的方法。 方法: 通过分析反应液pH、反应温度和原料比对玉竹多糖铁的性状及铁含量的影响,优化玉竹多糖铁配合物的合成工艺并采用间接碘量法测定铁含量。 结果: 以反应液pH 10~11,反应温度70~75 ℃,玉竹多糖与FeCl₃·6H₂O的质量比为1∶1.7作为合成工艺的优化条件,经优化条件合成的玉竹多糖铁具有很好的水溶性和稳定性。铁含量的3次测定值分别为20.0%,19.1%,21.8%,平均含量为20.0%,RSD为0.10%。 结论: 实验所确定的玉竹多糖铁配合物的优化合成工艺科学、简单、可靠。间接碘量法是测定玉竹多糖铁中铁含量的简便而可靠的方法。

Objective: To optimize the process of preparation protocol of Polygonatum odoratum(Mill.) Druce polysaccharide-Fe(Ⅲ) complex and establish the assay method of Fe (Ⅲ). Method: The influences of factors including pH,reaction temperature and proportion of starting materials on complex quality and assay of Fe(Ⅲ) were analyzed and the assay of Fe(Ⅲ) was done by the method of indirect iodimetry. Result: The optimized condition of the preparation were the pH of reaction solution was 10-11,the reaction temperature was 70-75 ℃,the mass ratio of Polygonatum odoratum(Mill.) Druce polysaccharide to FeCl₃·6H₂O was 1∶1.7.The complex synthesized with the optimized process was stable,with good solubility in water.the assay of Fe(Ⅲ) complex was 20.0%,19.1%,and 21.8%,average content was 20.0% with RSD of 0.10%. Conclusion: The established protocol for the preparation of Polygonatum odoratum(Mill.) Druce polysaccharide-Fe(Ⅲ) complex is scientific,convenient and reliable.The method of indirect iodimetry is reliable and stable in the determination of assay of Fe(Ⅲ) in Polygonatum odoratum(Mill.) Druce polysaccharide-Fe(Ⅲ) complex.

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