GC法测定羟乙基淀粉摩尔取代度的研究

目的对气相色谱法(GC)测定羟乙基淀粉摩尔取代度进行研究。方法色谱柱为DB-624石英毛细管柱(L=60 m,=0.53 mm),FID检测器;进样口温度为200℃,检测器温度为280℃;柱温采用程序升温,载气为氮气,流速为8 mL.min-1,分流比为1∶20。以甲苯为内标物。结果对照品碘乙烷在0.30～2.1 mg.mL-1(r=0.999 9)范围内呈良好线性关系。反应温度、时间对测定结果影响显著,最佳反应条件为135℃反应15 h;样品水分、氯化钠含量对测定结果无影响。结论该方法测定结果准确,简便快捷,适合羟乙基淀粉摩尔取代度的测定。

Study on the determination of molar substitution ratio of hydroxyethyl starch by GC

Objective To investigate the determination of molar substitution ratio of hydroxyethyl starch by GC. Methods The chromatographic system consisted of DB- 624 silica capillary column（ L = 60 m, Ф = 0.53 mm） and FID detector. The inlet temperature was 200℃ ,the detector temperature was 280 ℃ and temperature programming was used. The flow rate of N2 was 8 mL · rain ^- 1 with split ratio of 1 ： 20. Toluene was used as internal standard. Results The linearity of ethyl iodide was O. 30 - 2.1 mg · mL ^- 1 （ r= 0. 999 9 ） .The temperature and time had a significant effect on the results, of which the optimum condition was reaction at 135 ℃ for 15 h,while water and sodium chloride in the sample had no effect. Conclusion This method was accurate, convenient and suitable for the determination of molar substitution ratio of hydroxyethyl starch.