快速提取和分析马齿苋中五个三萜类化合物

Method for rapid extraction and analysis of five triterpenoids in P.oleracea

采用微波提取法提取了马齿苋中5个三萜类化合物,并利用三重四级杆串联线性离子阱质谱测定了这些成分的含量.开发的MWE-UPLC-MS/MS方法只需要10 min就可以提取马齿苋中的5个三萜类化合物,在11 min内就可对这些三萜类化合物进行定量分析.此外该方法也可大量减少溶剂消耗.验证数据表明,微波提取法结合UPLC-MS/MS技术是个十分可靠和稳定的分析方法.采用单因素实验考查了微波提取法的最优条件为:提取溶剂为甲醇、提取温度为70℃,提取时间为10 min,固液比为30 mL/g.验证结果表明该方法显示良好的线性、灵敏度、精确度、重现性和准确度.在本文中,一个MWE-UPLC-MS/MS方法被用于5个三萜类化合物的提取和定量,包括:熊果酸(1),2α,19α-二羟基熊果酸(2),3α,19α-二羟基熊果酸(3),19α,14-二羟基熊果酸(4),3-乙酰氧基油桐酸(5).该方法不仅可用于不同产地及不同采摘期的马齿苋,而且也可以应用于提取和测定其他复杂系统中的三萜类化合物.本次实验研究结果表明,不同生产区域的样品中5个三萜类化合物的含量差别很大.这些药物活性成分含量的测定对于马齿苋药效物质基础研究提供了很有价值的信息.

The optimal conditions of MWE for the extraction of triterpenes from P.oleracea involved the use of methanol as the extraction solvent.The experimental development of MWE-UPLC-MS/MS method requires only 10 minutes purslane can be extracted in 5 triterpenoids,only can these triterpenoids quantitatively analyzed in 11 minutes.In addition,the method can also be a significant reduction in solvent consumption.Verification data indicated that microwave extraction method with UPLC-MS/MS technique was very reliable and stable method of analysis.Determination of the concentration of active ingredients of these drugs for purslane quality assessment and clinical applications provide valuable information.A extraction temperature of 70℃,an extraction time of 10 min,and a solvent-to-solid ratio of 30 mL/g.The samples were analysed using an Ltra-performance liquid chromatograph coupled with a triple quadrupole-linear ion trap mass spectrometer(UPLC-MS/MS)system to quantify five triterpenes in P.oleracea from different sources.The results from the method validation study showed satisfactory linearity,sensitivity,accuracy,precision,reproducibility,and recovery for all five triterpenes.In this paper,a MWE-UPLC-MS/MS method was used for the extraction and quantification of five triterpenoids,including:ursolic acid(1),2α,19α-dihydroxy ursolic acid(2),3α,19α-dihydroxy ursolic acid(3),19α,14-dihydroxy ursolic acid(4),3-acetoxy-tung acid(5).This method can be used not only from different areas and different picking purslane,but can also be applied to other complex systems of extraction and determination of triterpenoids our results demonstrate that differences in the content of samples were observed in different production regions.This valuable information concerning the concentration of these pharmacologically active constituents in P.oleracea will be of great importance for quality assessment and should,therefore,be useful in assisting clinical applications.