酵母β-(1,3)-D-葡聚糖羧甲基化的工艺优化
首发时间:2012-12-24
摘要:本文以酵母β-(1,3)-D-葡聚糖为原料,以氯乙酸为羧甲基化试剂,采用二次加碱法对其进行羧甲基改性。IR结果显示,酵母β-(1,3)-D-葡聚糖衍生物在1568 cm-1处出现-COO-离子的新吸收峰,在 1414 cm-1处出现与羧基相连的次甲基-CH2-的吸收峰,表明羧甲基基团(-CH2COOH)已成功键接到β-(1,3)-D-葡聚糖分子链上。通过单因素试验研究反应温度、时间、NaOH用量、氯乙酸用量对取代度、黏度和溶解度的影响,并通过4因素3水平的正交试验对酵母β-(1,3)-D-葡聚糖羧甲基化工艺进行优化,得到的最佳羧甲基化反应条件为:反应温度50℃、反应时间5h、第一次加碱量为50%NaOH 4mL、第二次加碱量为50%NaOH 3mL、4mol/L氯乙酸15mL。在此最优工艺条件下进行羧甲基化得到的产物取代度为0.507±0.006,黏度为9.947±0.145Paos,溶解度为9.579±0.041mg/ml。
关键词: 酵母β-(1 3)-D-葡聚糖;羧甲基化;单因素试验;正交试验
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Processing Optimization for carboxymethylation of β-(1,3)-D-glucan from Yeast
Abstract:To utilize yeast (1→3)-β-D-glucan as biological response modifiers (BRMs) with better water solubility, carboxymethylation was carried out by a two-step alkalization and etherification with monochloroacetic acid. Carboxymethyl derivative was confirmed in FTIR spectra by three new strong absorption bands at 1568 cm-1 due to -COO- stretching vibrations, 1414 cm-1 of -CH2-, and 1046 cm-1 of -C-O-H. Four technological parameters of carboxymethylation were investigated by orthogonal experiments for obtaining the maximum degree of substitution (DS), apparent viscosity (η), and solubility (S) of carboxymethyl derivatives. In view of the orthogonal analysis, the optimal technological parameters were reaction temperature 50 C, total reaction time 5 h, 3 mL of 50% sodium hydroxide as the second alkali dosage, and 15 mL of 4 M chloroacetice acid. Under the optimal conditions, the value of DS、η and S were 0.507±0.006、9.947±0.145 Paos and 9.579±0.041mg/ml respectively.
Keywords: Yeastβ-1,3-glucan carboxymethylation single factor experiments orthogonal experiments
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