顶空毛细管气相色谱法测定辣椒碱中有机溶剂的残留量

Determination of Residual Solvents in Capsicine by Headspace Capillary GC

目的：建立顶空毛细管气相色谱法测定辣椒碱的有机溶剂残留量。方法：以（5%）苯基-（95%）甲基聚硅氧烷为固定液的毛细管柱为色谱柱,检测器为氢火焰离子化检测器（FID）,载气为氮气,顶空进样,采用外标一点法测定辣椒碱中甲醇、乙醇、乙酸乙酯、正己烷和正戊烷的有机溶剂残留量。结果：各有机溶剂的主峰均能良好分离,精密度RSD均小于10.0%,各溶剂在相应的浓度范围内有良好的线性关系,相关系数均不小于0.99,平均加样回收率均在80.0%~100.0%,并且其RSD均小于10.0%。结论：本方法专属性强、准确度高,可用于辣椒碱原料药中有机溶剂残留量的测定。

Objective： To establish a headspace capillary GC method for the determination of residual organic solvents of capsicine. Methods： The determination of residual organic solvents of capsicine was measured by capillary column [Phenyl-methyl polysiloxane（5 ： 95） as stationary liquid], using FID as detector, nitrogen as carrier gas, and one point external standard method was adopted to check the residues of methanol, ethanol, ethyl acetate petroleum ether. Results： The main peaks of organic solvents were well-separated, RSDs were all less than 10.0%, each solvent had a good linear relationship in the appropriate concentration range. The correlation coefficient was on less than 0.99, the average recoveries were 80.0%-100.0%, and RSDs were less than 10.0%. Conclusion： This method had strong specificity and high accuracy, and can be used in the determination of residual organic solvents of capsicine.