摘要
目的:筛选狼毒大戟抗肿瘤活性馏分,分离活性单体化合物并对构效关系进行探讨。利用超高效液相色谱-质谱联用技术(UPLC-Q-TOF-MS)对活性馏分的化学成分进行鉴定。方法:采用噻唑蓝(MTT)法对狼毒大戟乙醇提取物的石油醚、乙酸乙酯、正丁醇和水萃取部位的抗肿瘤活性进行测试。综合运用多种现代色谱分离手段对活性萃取层石油醚层进行分离。利用核磁(NMR)和质谱(MS)技术鉴定化合物的化学结构。质谱使用ESI离子源,正离子模式下采集数据,结合狼毒大戟相关文献以及对照品信息进行数据分析,解析活性馏分的化合物结构。结果:从活性馏分层石油醚层分离得到6个单体化合物,分别为岩大戟内酯A,岩大戟内酯B,17-羟-岩大戟内酯A,17-羟-岩大戟内酯B,euphopilolide,atis-16-en-13(s)-hydroxy-3,14-dione。对这些化合物的抗肿瘤活性的构效关系进行了探讨。利用UPLC-Q-TOF-MS对狼毒大戟乙醇提取物的石油醚萃取部位化学成分进行鉴定,共鉴定化合物23个,其中二萜类成分19个,酚类成分2个,脂肪酸类成分1个,三萜类成分1个。峰18和峰21初步鉴定为新化合物。结论:狼毒大戟的活性馏分层为石油醚层,其主要成分为二萜类,具有较好的抗肿瘤活性。UPLC-Q-TOF-MS技术能够快速准确地鉴定狼毒大戟活性馏分的化学成分结构,为其质量评价和活性物质基础研究提供了参考。
Objective:To screen out active fraction from Euphorbia fischeriana,separate active components from E.fischeriana and explore structure-activity relationships,in order to analyze and identify chemical compositions of petroleum ether fraction from E.fischerian ethanol extract by ultra-performance liquid chromatography with quadrupole-time-of flight mass spectrometry(UPLC-Q-TOF-MS).Method:The anti-tumor activities of petroleum ether,ethyl acetate,n-butanol and water extracts from E.fischeriana were tested by methyl thiazolyl tetrazolium(MTT)method.A variety of modern chromatographic separation methods were used to separate active compounds from petroleum ether layer.Compounds were isolated.Their structures were identified by NMR technique.The structure-activity relationships between anti-tumor activities and structures of compounds were investigated.UPLC-Q-TOF-MS technique was used to identify the structures of petroleum ether extract from E.fischeriana.Mass spectrometry was performed in the positive ion mode using ESI ion sources.Result:Six compounds were isolated from petroleum ether fraction.They were jolkinolide A,jolkinolide B,17-hydroxyjolkinolide A,17-hydroxyjolkinolide B,euphopilolide and atis-16-en-13(s)-hydroxy-3,14-dione.A total of 23 peaks were identified based on the comparison of retention times,accurate masses and fragmentation patterns with available standard compounds and literatures.Among them,there were 19 diterpenoids,2 polyphenols,1 fatty acid and 1 triterpenoid.Peaks No.18 and No.21 were tentatively identified as new compounds.Conclusion:The petroleum ether fraction showed a potential anti-tumor activity.The structure-activity relationships were discussed.UPLC-Q-TOF-MS technology can be used to quickly and accurately identify the structures,so as to provide a reference for its quality evaluation and active ingredient research.
作者
马玉坤
马天成
孙宇
刘雷
郭丽娜
孙珈
刘琦
韩翠翠
MA Yu-kun;MA Tian-cheng;SUN Yu;LIU Lei;GUO Li-na;SUN Jia;LIU Qi;HAN Cui-cui(Qiqihar Medical University,Qiqihar 161006,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2020年第7期156-164,共9页
Chinese Journal of Experimental Traditional Medical Formulae
基金
黑龙江省教育厅科学技术研究项目(2017-KYYWF-0702).
关键词
狼毒大戟
抗肿瘤活性
二萜类成分
乙醇提取物
石油醚萃取部位
Euphorbia fischeriana
antitumor activities
diterpenoids
ethanol extract
petroleum ether fraction
