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作 者:邓晓磊[1] 张建华[1] 周金娥[1] 陈泽乃[1] 陆阳[1]
出 处:《上海交通大学学报(医学版)》2008年第11期1398-1401,共4页Journal of Shanghai Jiao tong University:Medical Science
基 金:教育部高等学校博士点基金(20070248067);上海市教委基金(06BZ009)~~
摘 要:目的对玉米多糖铁的制备工艺进行优化并确立铁含量的测定方法。方法在制备玉米多糖铁的过程中,观察和分析反应液pH值、反应温度和投放原料比例对产品性状及铁含量的影响。根据分析结果优化制备工艺,并应用优化的制备工艺合成玉米多糖铁,观察其稳定性,同时采用滴定分析法(间接碘量法)测定铁含量,并以相对标准差(RSD)判别测定方法的可靠性和稳定性。结果经观察和分析,以反应液pH值11.0,反应温度65℃~75℃,玉米多糖(干重)与FeCl,·6H_2O的质量比值为1:1.7作为制备工艺的优化条件,经优化所合成的玉米多糖具有良好的水溶性和稳定性,3批产品的铁含量分别为39.86%、40.20%和40.17%。以间接碘量法测定铁含量的RSD<0.2%。结论实验所建立的玉米多糖铁优化制备工艺方法简单、可靠,适合工业生产。滴定分析是测定玉米多糖铁中铁含量的稳定且可靠的方法。Objective To optimize the preparation protocol of corn polysaccharide-Fe ( Ⅲ ) complex and establish the method of assay of Fe( Ⅲ). Methods During the preparation of corn polysaccharide-Fe( Ⅲ ) complex, the influences of factors including pH, reaction temperature and proportion of starting materials on product quality and assay of Fe(Ⅲ) were observed and analysed. The corn polysaccharide-Fe( Ⅲ) complex was prepared by the optimized preparation protocol with the analytic result. The stability of corn polysaccharide-Fe( Ⅲ ) complex was observed, the assay of Fe (Ⅲ) was done by the method of titrimetric analysis, and the reliability and consistency of the method were dertermined by relative standard deviation (RSD). Results The optimized conditions of preparation were 〉 11.0 for the pH of reaction solution, 65℃~ 75℃ for the reaction temperature, and 1:1. 7 for the mass ratio of corn (dry weight) to FeCl3 .6H2O. The corn polysaccharide-Fe( Ⅲ ) complex synthesized with the optimized process was stable, with good solubility in water. The assay of Fe( Ⅲ ) was 39.86% , 40.20% and 40.17% , respectively for three batches of products. The RSD was 〈0.2% for the titrimetric analysis of assay of Fe(Ⅲ). Conclusion The established protocol for the preparation of corn polysaccharide- Fe(Ⅲ) complex is convenient and reliable, and is suitable for mass production. The method of titrimetric analysis is reliable in the determination of assay of Fe( Ⅲ ) in corn polysaccharide-Fe(Ⅲ ) complex.
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