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目的制备褐藻酸钠系列降解产物,并建立其分子量的高效液相色谱(HPLC)检测方法。方法采用高压酸解法制备系列低分子量的褐藻酸钠的降解产物,并采用超滤分级法得到6种分子量的褐藻酸钠,用HPLC对褐藻酸钠的分子量进行分析。结果褐藻酸钠分级产物的色谱图中均只有一个吸收峰,峰宽较窄,峰形对称,表明分级效果较好,分子量较集中,可以用作褐藻酸钠标准品。以标准品的分子量对数(logMw)对保留时间(t)进行回归处理,得到线性回归方程:logMw=-0.711 9t+15.713,R=0.971,回归关系较好,批间变异系数<5%,表明方法的重现性较高。结论本研究为褐藻酸钠分子量测定制备了标准品并建立了HPLC检测方法,为褐藻酸钠分子量的测定工作提供了实践依据。
Objective To prepare a series of degradation products of sodium alginate and establish a high performance liquid chromatography (HPLC) detection method for its molecular weight. Methods A series of low molecular weight sodium alginate degradation products were prepared by high pressure acid hydrolysis. Six kinds of sodium alginate were obtained by ultrafiltration and fractionation. The molecular weight of sodium alginate was analyzed by HPLC. Results There were only one absorption peak in the chromatogram of the sodium alginate fractionation product. The peak width was narrow and the peak shape was symmetrical, indicating that the classification effect was good and the molecular weight was more concentrated. It could be used as a sodium alginate standard product. The logarithm of the logarithm of the standard (logMw) on the retention time (t) was subjected to regression processing to obtain the linear regression equation: logMw=-0.711 9t+15.713, R=0.971, the regression relationship was good, and the inter-assay coefficient of variation was <5%. This shows that the method is more reproducible. Conclusion This study prepared a standard product for molecular weight determination of sodium alginate and established a HPLC detection method, which provided a practical basis for the determination of sodium alginate molecular weight.