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ASE-HPLC-PDA-ESI-ITMSn法分析甘遂中的二萜类成分

Analysis of Diterpenes in Radix Kansui by ASE-HPLC-PDA-ESI-ITMS^n
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摘要 目的建立加速溶剂萃取法(ASE)提取甘遂二萜类成分的最优提取工艺,并定性鉴别提取物中的二萜类成分。方法在单因素试验考察萃取溶剂、温度、时间和循环次数对提取率影响的基础上,采用响应面分析法对提取工艺参数进行优化,并与传统提取方法进行比较。利用高效液相色谱-光电二极管阵列检测器-电喷雾离子阱多级质谱(HPLC-PDA-ESI-ITMSn)对提取物进行定性分析。结果加速溶剂萃取法提取甘遂二萜类成分的最优提取工艺为:以乙醇为提取溶剂,提取温度110℃,提取时间13 min,循环3次。通过HPLC-PDAESI-ITMSn鉴别出53个二萜类化合物,包括40个巨大戟二萜醇类二萜和13个假白榄酮型二萜。结论与传统提取方法相比,加速溶剂萃取法能最大程度地提取甘遂中的二萜类成分,具有操作简单方便、省时高效、安全环保等优点。 Objective To establish an optimal accelerating-solvent extraction (ASE) method for the extraction of diterpenes from Radix Kansui. Methods A response surface methodology (RSM) on the basis of single factor experiment was adopted to optimize extraction solvent, extraction temperature, extraction time and static cycle. Afterwards, a comparison among ASE and traditional extraction was carried out. The diterpenes in the ASE extracts of Radix Kansui were identified by HPLC-PDA-ESI-ITMSn. Results The optimum extraction conditions were as follows: with ethanol as the extraction solvent, extraction temperature was set at 110 ~C, extraction time was 13 min and the extraction lasted 3 static cycles. By using HPLC-PDA-ESI-ITMS", 53 diterpenes constituents were identified, including 40 ingenol type diterpenes and 13 jatrophone type diterpenes. Conclusion The yield of diterpenes fromRadix Kansui extracted by ASE method under the optimum conditions is significantly higher than that by traditional extraction method. ASE method is a simple, quick, effective, environment-protecting method for extracting the diterpenes from Radix Kansui.
出处 《中药新药与临床药理》 CAS CSCD 北大核心 2015年第4期517-525,共9页 Traditional Chinese Drug Research and Clinical Pharmacology
基金 上海市药物(中药)代谢产物研究重点实验室开放课题(2012SHDX1002)
关键词 甘遂 二萜 加速溶剂萃取 响应面分析 高效液相色谱-光电二极管阵列检测器-电喷雾离子阱多级质谱 Radix Kansui Diterpenes Accelerating solvent extraction Response surface methodology HPLC-PDA-ESI-ITMSn
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