UPLC-MS/MS分析及NMR技术鉴定千金子中二萜类化合物

Identification of Diterpenoids from Euphorbiae Semen by UPLC-MS/MS and NMR

目的:研究千金子乙酸乙酯提取部分的二萜成分。方法:利用乙醇回流提取法进行提取,超高效液相色谱-质谱法(UPLC-MS/MS)结合对照品分析千金子乙酸乙酯部分化学成分;用硅胶和Sephadex LH-20型葡聚糖凝胶色谱技术进行分离;用核磁共振法对化合物12进行结构鉴定。结果:千金子乙酸乙酯提取部分的12个化合物分别鉴定为千金子素(euphorbia factor,EF)L25(1)、EFL1(2)、EFL13(3)、EFL7b(4)、EFL12/EFL12异构体(5)、EFL18(6)、EFL17(7)、EFL3(8)、EFL7a(9)、EFL23(10)、EFL11(11)、EFL2(12)。结论:基于对照品的UPLC-MS/MS结合传统提取分离法是用于研究千金子乙酸乙酯提取部分化学成分的有效方法。

Objective:To study the diterpenoids from ethyl acetate extract of Euphorbiae Semen.Methods:The medicinal was extracted by ethanol reflux,and the components in ethyl acetate extract were analyzed by ultra performance liquid chromatography with tandem mass spectrometry(UPLC-MS/MS)with reference samples.Sephadex LH-20 chromatography and silica gel column chromatography were employed for separation.Furthermore,the structure of compound 12 was confirmed by nuclear magnetic resonance(NMR).Results:Twelve diterpenoids were identified from ethyl acetate extract of Euphorbiae Semen as euphorbia factor(EF)L25(1),EFL1(2),EFL13(3),EFL7b(4),EFL12/EFL12 isomer(5),EFL18(6),EFL17(7),EFL3(8),EFL7a(9),EFL23(10),EFL11(11),and EFL2(12),respectively.Conclusion:Combination of UPLC-MS/MS and traditional purification is a powerful means for investigating the chemical ingredients of ethyl acetate extract of Euphorbiae Semen.