金银花水提醇沉工艺过程回收乙醇中杂质的定性及合规分析

Qualitative and Compliance Analysis of Impurities in the Ethanol Recovered from Ethanol Deposition Solution of Aqueous Extract of Lonicerae Japonicae Flos

关键词:  金银花  回收乙醇  杂质定性  合规分析

Key words:  Lonicerae Japonicae Flos  ethanol recovery  impurity characterization  compliance analysis

摘要:

目的 探究回收乙醇套用次数对金银花水提醇沉工艺过程回收乙醇质量的影响。方法 减压蒸馏回收5个连续批次金银花水提醇沉液中的乙醇，采用顶空固相微萃取-气相色谱/质谱(HS-SPME/GC-MS)方法定性分析5批回收乙醇及温度失控产生局部焦化时回收乙醇中的杂质，并对各批回收乙醇进行紫外吸光度分析。结果 第1，2批回收乙醇中杂质仅有苯乙烯；第3，4批回收乙醇杂质为5种；第5批回收乙醇中杂质种类增加到17种；产生局部焦化时回收乙醇中外源性杂质剧增至41种并产生茚类和萘类等有害物质。第3~5批回收乙醇的紫外吸光度超过中国药典2020年版二部规定的乙醇紫外吸光度上限，局部焦化时回收乙醇的紫外吸光度严重超出药典规定的范围。结论 水提醇沉过程回收乙醇连续套用2次后应进行处理，使其紫外吸光度水平与杂质种类达到新鲜乙醇要求，方可再次使用，该方法对回收乙醇的质量监控和合规应用提供了参考。

Abstract:

OBJECTIVE To explore the influence of reusing and recycling times on the quality of ethanol recovered from ethanol deposition solution of aqueous extract of Lonicerae Japonicae Flos. METHODS The ethanol in five consecutive batches of Lonicerae Japonicae Flos water extract ethanol deposition was recovered by vacuum distillation. The impurities in five batches of recovered ethanol and the recovered ethanol when partial coking caused by temperature runaway were qualitatively analyzed by headspace solid phase micro extraction combined with gas chromatography-mass spectrometry(HS-SPME/GC-MS), and the ultraviolet absorbance of each batch of recovered ethanol was also analyzed. RESULTS Styrene was the only impurity in the first and second batch of recovered ethanol; there were five impurities in the third and fourth batch of recovered ethanol; the number of impurities in the fifth batch of recovered ethanol increases to 17. When partial coking was occurred, the exogenous impurities in the recovered ethanol increased dramatically to forty-one, and there were harmful substances such as ninhydrin and naphthalene. The ultraviolet absorbance of the third to fifth batch of recovered ethanol exceed the upper limit stipulated in the second part of Chinese Pharmacopoeia, 2020 Edition. While the ultraviolet absorbance of the recovered ethanol when partial coking takes place exceeds the standard of the pharmacopoeia greatly. CONCLUSION The recovered ethanol should be treated after being reused two times, so that its ultraviolet absorbance level and impurity type are equivalent to that of fresh ethanol before it can be used again. The method provides reference for the quality control and compliance use of recovered ethanol.