[关键词]
[摘要]
目的 建立中药生产过程乙醇精制后质量评价方法,评估精馏乙醇再利用的可能性。方法 以天津天士力之骄药业有限公司五味子提取过程中用的乙醇经回收、精制得到的精馏乙醇为例,采用气相-质谱法(GC-MS)、液相-质谱(LCMS)法、气相色谱(GC)法、超高效液相色谱(UPLC)法、紫外-可见分光光度法等多个分析手段,评价精馏乙醇与相应新醇质量的差异,评估精馏乙醇的再利用风险,建立精馏乙醇的质量控制指标。结果 采用GC-MS、GC方法,对挥发性杂质分析,GC-MS发现新的杂质,由于含量低,在GC中未检出;采用LC-MS、UPLC、吸光度方法,对不挥发性杂质综合分析,有个别批次UPLC方法可检出新的杂质,为控制新增未知杂质,筛选一个低毒、出峰时间适宜、且与乙醇中各色谱峰分离度较好的苯乙烯作为对照物,建立未知峰的半定量液相测定方法及限制,用于日常的质量控制。结论 通过多维度质量评价及风险评估,建立精馏乙醇质量评价模式。
[Key word]
[Abstract]
Objective To establish the quality evaluation method of the refining ethanol in the extraction process of traditional Chinese medicine and to evaluate the possibility of reuse of the refining ethanol. Method Taking the ethanol used in the process of extracting Schisandra chinensis from Tianjin Tasly Pride Pharmaceutical Co., Ltd. as an example. Evaluate the difference between the quality of refining ethanol and the corresponding fresh ethanol by the methods of Gas chromatography-mass spectrometry, liquidmass spectrometry, gas chromatography, liquid chromatography, UV-Vis spectrophotometry and so on, and to evaluate the risk of reuse of refining ethanol. Establish quality specification of refining ethanol. Results GC-MS and GC methods were used to analyze volatile impurities. New impurities were found in GC-MS, but they were not detected in GC due to their low content; LC-MS, UPLC and absorbance methods were used for comprehensive analysis of non-volatile impurities, and some batches of UPLC method could detect new impurities. In order to control the new unknown impurities, a low toxicity, suitable peak time, and the resolution of each chromatographic peak in ethanol was selected. The method and limit of semi quantitative liquid phase determination of unknown peak were established for routine quality control. Conclusion Establish the model of refining ethanol quality evaluation through multi-dimensional quality evaluation and risk assessment.
[中图分类号]
R926
[基金项目]
天津市科技计划项目(18YFCZZC00430)