顶空气相色谱法测定水杨酸甲酯乳糖苷中残留溶剂研究

Study on Determination of Residual Solvents in Methyl salicylate-2-O-β-D-galactopyranoside (1-4)-β-D- glucopyranoside by Head-space Capillary Gas Chromatography

目的建立了测定水杨酸甲酯乳糖苷中甲醇、乙醇、二氯甲烷、乙酸乙酯有机溶剂含量的顶空气相色谱法。方法采用顶空气相色谱法,FID检测器,以二甲基亚砜为溶媒,顶空预热温度为90℃,预热时间为30min,进样口温度为250℃,检测器温度为250℃,以氦气为载气,使用DB-624交联毛细管柱(30m×0.53mm,i.d,3μm),采用程序升温,实现了各组分的基线分离。结果甲醇、乙醇、二氯甲烷及乙酸乙酯在各自对应的浓度范围内,线性关系良好;甲醇、乙醇、二氯甲烷、乙酸乙酯的最小检测限分别为0.35μg/mL、0.61μg/mL、0.52μg/mL、0.54μg/mL;加样回收率均在95%以上,精密度良好。结论经方法学验证,该方法灵敏、准确、可靠,可适用于水杨酸甲酯乳糖苷中甲醇、乙醇、二氯甲烷及乙酸乙酯残留有机溶剂的测定。

Objective This paper reports a Head-space GC method for determination of methanol,enthanol,dichloromethane,ethylac etate in MSG.Method The analytical column was DB-624 （ 30m× 0.53mm,i.d,3μ m ） . The injector temperature was 250℃ and the detector temperature was 250%.The column temperature was programmed raised. The carrier gas was helium and the solvent was dimethyl sulfoxide.Resu Its The stand curve was linear for each solvent in the range of each consistency.The average recoveries were all more than 95%.Conclusion This method is simple,rapid and precise;it is suitable for measurement of residual solvents in MSG.