热重-气质联用法快速鉴别熊果酸对照品原料中残留溶剂

Rapid identification of residual solvent in ursolic acid raw material by thermo gravimetric analysis-gas chromatography-mass spectrometry

中药化学对照品原料通常经由提取分离纯化制备而获取,因而容易存在有机残留溶剂。以熊果酸对照品原料为例,利用热重分析-气相色谱-质谱联用技术,建立了对照品原料中残留溶剂的快速鉴别检测方法。熊果酸对照品原料直接放置热重分析仪天平上,通过热重分析-气相色谱-质谱联用仪采用梯度升温程序进行在线检测,经一级与二级质谱分析鉴定其中的残留溶剂为乙醇。结果表明,该方法能够快速鉴别熊果酸对照品原料中的残留溶剂乙醇。

Traditional Chinese medicine chemical reference standards are generally obtained by the process from extraction and purification for preparation, which will cause the organic residual solvents. A rapid identification method for residual solvent in ursolic acid reference standard raw materials was established by using thermo gravimetric analysis-gas chromatography-mass spectrometry （TGA-GC-MS） coupled instrument. Ursolic acid raw materials were directly placed on the balance of the thermo gravimetric analyzer, and measured by TGA-GC-MS through gradient heating program. The residual solvent was identified as ethanol by analysis of the primary and secondary mass spectra. The results showed that the method could rapidly identify the residual solvent ethanol in ursolie acid raw material. The hyphenated method was accurate, simple, effective, and environment-friendly. It＇s suitable for accurate and rapid screening of residual solvents in the raw materials of TCM chemical reference standards.