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建立气相色谱-串联质谱法对药用甘油中二聚甘油谜进行定性、定量分析。气相色谱条件,色谱柱:Rxi-5ms,0.25μm×30.0m×0.25mm,高纯氦气,进样口温度:200℃,流速:1.23ml/min,柱温:起始温度为100℃,保持4min,再以50℃/min的速度升至120℃,保持10min,接着以50℃/min的速度升至200℃,保持6min,进样模式:不分流。质谱条件:离子源温度200℃,溶剂延迟时间3min,EI电离源,扫描范围:35-300amu。得到了样品总离子流图及各相应的质谱图,对其进行解析,初步鉴定出药用甘油中的有关物质二聚甘油醚为化合物3、4、5。本方法为研究药用甘油中环状二聚甘油谜为用药安全和提高产品质量提供了科学依据。
Gas chromatography-tandem mass spectrometry (GC-MS / MS) was established for the qualitative and quantitative analysis of diglycerol enolysis in medicinal glycerol. GC conditions: Rxi-5ms, 0.25μm × 30.0m × 0.25mm, high purity helium, inlet temperature: 200 ℃, flow rate: 1.23ml / min, column temperature: initial temperature of 100 ℃, Maintain 4min, and then 50 ℃ / min speed rose to 120 ℃, hold 10min, then 50 ℃ / min speed rose to 200 ℃, hold 6min, injection mode: split. MS conditions: ion source temperature 200 ℃, solvent delay time 3min, EI ionization source, scanning range: 35-300amu. The total ion chromatogram and the corresponding mass spectra of the sample were obtained. The analytical results of the sample showed that the diglycerol ether in the medicinal glycerol was compound 3,4,5. The present method provides a scientific basis for studying drug safety and product quality in the study of cyclic glycidol in medicinal glycerol.