目的 建立中藥生產(chǎn)過程乙醇精制后質(zhì)量評價方法，評估精餾乙醇再利用的可能性。方法 以天津天士力之驕藥業(yè)有限公司五味子提取過程中用的乙醇經(jīng)回收、精制得到的精餾乙醇為例，采用氣相-質(zhì)譜法（GC-MS）、液相-質(zhì)譜（LCMS）法、氣相色譜（GC）法、超高效液相色譜（UPLC）法、紫外-可見分光光度法等多個分析手段，評價精餾乙醇與相應(yīng)新醇質(zhì)量的差異，評估精餾乙醇的再利用風險，建立精餾乙醇的質(zhì)量控制指標。結(jié)果 采用GC-MS、GC方法，對揮發(fā)性雜質(zhì)分析，GC-MS發(fā)現(xiàn)新的雜質(zhì)，由于含量低，在GC中未檢出；采用LC-MS、UPLC、吸光度方法，對不揮發(fā)性雜質(zhì)綜合分析，有個別批次UPLC方法可檢出新的雜質(zhì)，為控制新增未知雜質(zhì)，篩選一個低毒、出峰時間適宜、且與乙醇中各色譜峰分離度較好的苯乙烯作為對照物，建立未知峰的半定量液相測定方法及限制，用于日常的質(zhì)量控制。結(jié)論 通過多維度質(zhì)量評價及風險評估，建立精餾乙醇質(zhì)量評價模式。

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.

R926

天津市科技計劃項目（18YFCZZC00430）