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目的:建立毛细管气相色谱法(CGC法)检测榄香烯原料药的有关物质。方法:采用DB-WAXetr(60 m×0.32 mm×0.25μm)毛细管气相色谱柱,柱温为程序升温(起始柱温为80℃,维持5 min,以3℃·min~(-1)的速率升温至185℃,再以20℃·min~(-1)的速率升温至230℃,维持60 min),进样口温度230℃,检测器温度230℃,分流比为10:1,进样量1.0μL。结果:方法的专属性强,β-榄香烯质量浓度在5.003 6~160.12μg·mL~(-1)的范围内呈线性(r=1.000 0,n=7),最低检出限为0.87μg·mL~(-1);3批样品的有关物质总量依次为15.4%、15.5%、14.7%。结论:本方法可用于榄香烯原料药的有关物质检测。
Objective: To establish a capillary gas chromatography (CGC method) for the determination of elemene related substances. Methods: The capillary column of DB-WAXetr (60 m × 0.32 mm × 0.25 μm) was used. The temperature of the column was programmed to increase (the initial column temperature was 80 ℃ and maintained for 5 min at 3 ℃ · min -1 The temperature was raised to 185 ° C, and the temperature was raised to 230 ° C at a rate of 20 ° C / min to maintain the temperature for 60 minutes. The temperature of the inlet was 230 ° C, the temperature of the detector was 230 ° C, the split ratio was 10: 1, The sample volume was 1.0 μL. Results: The method was highly specific. The mass concentration of β-elemene was linear (r = 1.000 0, n = 7) in the range of 5.003 6 ~ 160.12 μg · mL -1 with the lowest detection limit of 0.87 μg · mL -1. The total amount of related substances in three batches of samples was 15.4%, 15.5% and 14.7%, respectively. Conclusion: This method can be used for the detection of substances related to elemene.