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目的:建立毛细管气相色谱法测定药用辅料倍他环糊精中的残留溶剂。方法:采用顶空气相色谱法测定,色谱柱为DB-1石英毛细管柱(50 m×0.53 mm,5μm),载气为氮气。进样口温度为200℃,FID检测器,检测器温度为250℃,柱温为90℃,顶空进样,平衡温度为70℃,平衡时间为20 min,分流比为1:1;20%二甲基亚砜溶液为溶剂;二氯乙烯为内标物。结果:被测物得到很好分离,峰面积与浓度呈良好线性关系,精密度和回收率良好。结论:该方法可用于倍他环糊精中残留溶剂的检测。
Objective: To establish a capillary gas chromatographic method for the determination of residual solvents in the pharmaceutical excipient beta-cyclodextrin. Methods: The sample was determined by headspace gas chromatography. The column was DB-1 quartz capillary column (50 m × 0.53 mm, 5 μm). The carrier gas was nitrogen. Inlet temperature was 200 ° C, FID detector, detector temperature was 250 ° C, column temperature was 90 ° C, headspace injection, equilibrium temperature was 70 ° C, equilibration time was 20 min, split ratio was 1: 1; 20 % Dimethyl sulfoxide solution as solvent; dichloroethylene as internal standard. Results: The analytes were well separated, the peak area showed a good linear relationship with the concentration, and the precision and recovery were good. Conclusion: This method can be used for the determination of residual solvent in beta cyclodextrin.