D-氨基葡萄糖硫酸盐水解条件的优化及组分分析

Hydrolysis condition optimization for D-glucosamine sulfate and composition analysis

采用响应面分析法对H_2SO_4水解壳聚糖制备D-氨基葡萄糖胺硫酸盐工艺参数进行了优化,探索提取时间(min)、提取温度(℃)、物料比(m L/g)和H_2SO_4质量分数对D-氨基葡萄糖硫酸盐得率的影响,建立了提取D-氨基葡萄糖硫酸盐的二次项数学模型,得到最优提取工艺参数,并采用高效液相色谱-质谱联用仪(HPLC-MS)对H_2SO_4水解壳聚糖制备的组分进行初步分析。研究结果表明:H_2SO_4水解壳聚糖制备D-氨基葡萄糖硫酸盐的最佳工艺条件为H_2SO_4质量分数53.29%、物料比(m L/g)6∶1、温度88.31℃、时间6 h,在此工艺条件下的D-氨基葡萄糖硫酸盐得率为43.86%。影响D-氨基葡萄糖硫酸盐得率的因素主次顺序为温度、时间、H_2SO_4质量分数、物料比。用HPLC-MS测定提取物,首次发现H_2SO_4水解壳聚糖可得到D-氨基葡萄糖硫酸盐、葡萄糖胺和葡萄糖胺二聚糖硫酸盐混合物。

The process parameters of D-glucosamine sulfate prepared from sulfuric acid hydrolysis of chitosan were optimized using the response surface analysis method,to explore the influences of extraction time（ min）,extraction temperature（ ℃）,material ratio（ mL/g） and sulfuric acid concentration on the yield of D-glucosamine sulfate. Meanwhile,a quadratic term mathematical model for extracting Dglucosamine sulfate was established to obtain the optimal extraction parameters.Components prepared from sulfuric acid hydrolysis of chitosan were preliminarily analyzed using HPLC-MS.The optimum conditions to prepare D-glucosamine sulfate from sulfuric acid hydrolysis of chitosan were as follows： sulfuric acid concentration of 53. 29%,material ratio（ mL/g） of 6 ∶ 1,temperature of 88. 31 ℃ and duration of 6 h.The yield of D-glucosamine sulfate under these conditions was 43. 86%.The primary and secondary sequences of factors affecting the yield of D-glucosamine sulfate were temperature,extraction time,sulfuric acid concentration,and material ratio in succession.The extract was determined using HPLC-MS,and we firstly found that sulfuric acid hydrolysis of chitosan could obtain the mixture of D-glucosamine sulfate,glucosamine and glucosamine disulfide sulfate.