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目的考察穿心莲内酯类成分在不同溶剂中的化学稳定性。方法以非极性、极性溶剂及不同体积分数的甲醇或乙醇为溶剂提取穿心莲内酯类成分,利用HPLC法检测其变化规律,探讨不同提取介质对其化学稳定性的影响。结果极性溶剂及醇水混合溶剂对穿心莲内酯类化学成分的提取率较高,但是介质极性增大会降低其化学稳定性;常温条件下,以甲醇为溶剂,穿心莲内酯、脱水穿心莲内酯和去氧穿心莲内酯在放置过程中含量逐渐升高,3 d后开始下降,在HPLC图谱中显示峰较明显的X1和X2成分则一直下降;在不同体积分数的甲醇-水溶液中,5个指标成分的含量一直下降;在乙醇、85%乙醇中,5个指标成分3 d内均较稳定,之后开始下降,但下降幅度较不同体积分数甲醇作溶剂时低。以85%乙醇为介质,经100℃加热30 min后穿心莲内酯、去氧穿心莲内酯和脱水穿心莲内酯的含量均升高,2 h后仅脱水穿心莲内酯仍升高,X1和X2一直降低;于-80℃放置12 h后,各内酯成分基本保持不变。结论穿心莲内酯类成分在乙醇和85%乙醇中稳定,在甲醇中不稳定,在甲醇-水中变化较大;穿心莲内酯类成分的化学稳定性较差,分析过程中应注意溶剂的选择,不宜长时间放置;穿心莲内酯和去氧穿心莲内酯的热稳定性较差,生产过程中应随时监测环境温度,尽量保持低温。
Objective To investigate the chemical stability of andrographolide in different solvents. Methods The constituents of andrographolide were extracted with non-polar, polar solvents and different volume fractions of methanol or ethanol. The changes of the andrographolide contents were detected by HPLC and the effects of different extraction media on their chemical stability were discussed. Results The extraction rate of the andrographolide from the polar solvent and alcohol-water mixed solvent was high, but the increase of the polarity of the medium decreased the chemical stability. Under normal temperature, methanol was the solvent, andrographolide The contents of ester and deoxyandrographolide increased gradually after 3 days and began to decline after 3 days. The components of X1 and X2 which showed obvious peaks in HPLC showed a decreasing trend. In different volume fractions of methanol-water solution, 5 The content of the index components decreased all the time. In the ethanol and 85% ethanol, the five index components were stable within 3 days, then began to decline, but the decrease rate was lower than the different volume fraction of methanol as the solvent. The contents of andrographolide and dehydroandrographolide were all increased after heated at 100 ℃ for 30 min with 85% ethanol as medium. After only 2 hours, the content of andrographolide was still increased, while the concentrations of andrographolide Lower; at -80 ℃ for 12 h, the content of each lactone remained unchanged. Conclusion The composition of andrographolide is stable in ethanol and 85% ethanol, unstable in methanol, and greatly changes in methanol - water. The chemical constituents of andrographolide are poor in chemical stability. During the analysis, the solvent selection, Should not be placed for a long time; Andrographolide and deoxy-andrographolide poor thermal stability, the production process should be monitored at ambient temperature, try to keep the temperature.