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齐齐哈尔医学院,黑龙江 齐齐哈尔 161006
[第一作者] 马玉坤,硕士,实习研究员,从事天然药物化学成分研究,Tel:0452-2663371,E-mail:769650146@qq.com
*孙宇,博士,助理研究员,从事天然药物化学成分及质量分析研究,Tel: 0452-2663371,E-mail:zsy5811321@126.com
收稿日期:2019-09-25,
网络出版日期:2019-10-11,
纸质出版日期:2020-04-05
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马玉坤, 马天成, 孙宇, 等. 狼毒大戟抗肿瘤活性成分[J]. 中国实验方剂学杂志, 2020,26(7):156-164.
Yu-kun MA, Tian-cheng MA, Yu SUN, et al. Anti-tumor Constituents from Rhizome of
马玉坤, 马天成, 孙宇, 等. 狼毒大戟抗肿瘤活性成分[J]. 中国实验方剂学杂志, 2020,26(7):156-164. DOI: 10.13422/j.cnki.syfjx.20200216.
Yu-kun MA, Tian-cheng MA, Yu SUN, et al. Anti-tumor Constituents from Rhizome of
目的:
2
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:
2
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:
2
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:
2
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:
2
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:
2
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:
2
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:
2
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.
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