顶空气相色谱法测定胡黄连苷Ⅱ原料药中7种有机溶剂残留量

Residual Determination of 7 Organic Solvents in PicrosideⅡRaw Material by Head-space GC

目的：建立测定胡黄连苷Ⅱ原料药中7种有机溶剂残留量的方法。方法：采用顶空气相色谱法。色谱柱为以6%氰丙基苯基-94%二甲基聚硅氧烷（DB-624）为固定液的毛细管柱,程序升温,进样口温度为200℃,检测器为氢火焰离子化检测器,温度为250℃,氮气流速为35 ml/min,分流比为10∶1,顶空进样量为1 ml,顶空加热温度为85℃,平衡时间为45 min。结果：甲醇、乙醇、乙酸乙酯、甲苯、苯、苯乙烯、二乙烯苯在各自质量浓度范围内与峰面积呈良好的线性关系（r为0.999 6~0.999 9）;精密度、稳定性试验的RSD〈3%;平均加样回收率为78.0%~104.9%,RSD分别为0.65%~2.47%（n=6）。结论：该方法专属性强,操作简便快速,结果准确,可用于胡黄连苷Ⅱ原料药中有机溶剂残留量的测定。

OBJECTIVE ： To establish the method for the residual determination of 7 organic solvents in picroside Ⅱ raw materi- als. METHODS： Head-space GC was performed on the capillary column of 6% cyanopropyl phenyl-94% dimethyl polysiloxane （DB-624） by temperature programming, the temperature of injector was 200 ℃, temperature of flame ionization detector was 250 ℃, the flow rate of N2 was 35 ml/min, and split ration was 10 ： 1, headspace sampling was adopted with the volume of 1 ml, the heating temperature of headspace sampling was 85 ℃, heating time was 45 min. RESULTS： The good linear relationship of methanol, ethanol, ethylacetate, methylbenzene, benzene, phenylethylene and divinglbenzene had been obtained （r = 0.999 6-0.999 9） ; RSDs of precision stability test were less than 3% ; average recoveries was in the range of 78.0%-104.9% （RSDs were 0.65%-2.47%, n=6）respectively. CONCLUSIONS： The method is specific, rapid, simple and accurate, and can be used for the determination of residual organic solvents in picroside Ⅱ raw materials.