响应面法优化海藻酸钠消化工艺及结构分析

doi:10.13218/j.cnki.csdc.2015.03.005

摘要/Abstract

摘要： 采用响应面试验设计和分析方法优化了从海南马尾藻中提取海藻酸钠的消化工艺,得到最佳消化工艺条件为:Na₂CO₃的质量分数为2.49%,消化温度为61.42 ℃,消化时间为2.07 h,预测最高提取率为34.99%,实测值为34.82%,相对误差仅为0.047 7%,模型拟合度很好。实验采用核磁共振氢谱(¹HNMR)对比表征和分析了从海南马尾藻中提取的海藻酸钠与市购海藻酸钠的甘露糖醛酸(M)和古罗糖醛酸(G)的比值及G,M,GG,GM,MM和MG片段的结构数据,其F_M/F_G值分别为0.41和1.72,说明两者结构相差较大;进而采用凝胶色谱法(GFC)测得市购海藻酸钠和自提海南马尾藻海藻酸钠分子量分别为488 699和93 766,分散系数(PDI)皆小于3,分子量分布较均匀;采用透射电子显微镜(TEM)分析观察了2种海藻酸钠在水溶液中的形态结构,结果发现结构及分子量不同的自提海藻酸钠在水溶液中呈线性网状交联分布,在0.15 mol/L NaCl溶液中能自组装形成分散均匀,粒径约为40 nm的聚集体,并用荧光光谱法测得其临界聚集浓度(cac)为0.884 7 g/L。

关键词: 化妆品添加剂, 海藻酸钠, 马尾藻, 响应面法, 结构

Abstract: Response surface method (RSM) was used to optimize technological parameters for digestion process of extraction of sodium alginate (SA) from Hainan wild sargassum.The optimum technical conditions were as follows:Na₂CO₃ mass fraction,2.49%;digestion temperature,61.42 ℃;digestion time,2.07 h.Under these conditions,the extraction yield of SA from Hainan wild sargassum could reach 34.82%,which is close to practical value 34.99%.The relative error was only 0.047 7%,showing that the model fits pretty well.¹HNMR was used to characterize and analyze the ratio of the mannuronic acid (M) to guluronic acid (G),the sequences and composition ratios of G,M,GG,GM,MM and MG of the prepared product and that of the market product.The F_M/F_G ratios of the prepared product and market product are 0.41 and 1.72 respectively,indicating a great difference of their structure.Meanwhile,molecular weight of the prepared product and the market product are 488 699 and 93 766 respectively,and all their polydispersity (PDI) are less than 3,indicating that the molecular weight distribution is rather uniform.Morphological structure of the prepared product and the market product was observed via TEM.And results showed that the prepared product with different structure and molecular weight is forming linear network crosslinking distribution in aqueous solution and self aggregating into spherical aggregates with a uniform dispersion and similar size of 40 nm in 0.15 mol/L NaCl aqueous solution.Its critical aggregating concentration was detected by photofluorimeter and the result value is 0.884 7 g/L.

Key words: additive of cosmetics, sodium alginate, sargassum, response surface method, structure

中图分类号:

TQ658

李可, 李嘉诚, 黄俊浩, 王荔宁, 张永利, 颜慧琼, 伍剑博. 响应面法优化海藻酸钠消化工艺及结构分析[J]. 日用化学工业, 2015, 45(3): 143-148.

LI Ke, LI Jia-cheng, HUANG Jun-hao, WANG Li-ning, ZHANG Yong-li, YAN Hui-qiong, WU Jian-bo. Response surface method as an approach for optimization of digestion process of sodium alginate and its structure analysis[J]. China Surfactant Detergent & Cosmetics, 2015, 45(3): 143-148.

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