中国中药杂志

2020, v.45(19) 4667-4676

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基于UPLC-Q-TOF-MS和UPLC-QQQ-MS/MS的东革阿里苦木素二萜成分分析
Qualitative and quantitative analysis of quassinoid diterpenoids from Eurycoma longifolia by UPLC-Q-TOF-MS combined with UPLC-QQQ-MS/MS

陈秀明;方东升;周璟明;郑孝贤;林斌;王海龙;詹清;
CHEN Xiu-ming;FANG Dong-sheng;ZHOU Jing-ming;ZHENG Xiao-xian;LIN Bin;WANG Hai-long;ZHAN Qing;Fujian Provincial Key Laboratory of Screening for Novel Microbial Products, Fujian Institute of Microbiology;

摘要(Abstract):

应用超高效液相色谱-串联四极杆飞行时间质谱(UPLC-Q-TOF-MS)和超高效液相色谱-三重四极杆串联质谱(UPLC-QQQ-MS/MS)对东革阿里提取物中的苦木素二萜成分进行定性和定量分析。UPLC-Q-TOF-MS采用Agilent Eclipse Plus C_(18) RRHD色谱柱(2.1 mm×100 mm,1.8μm),以乙腈-0.1%甲酸水为流动相进行梯度洗脱。UPLC-QQQ-MS/MS采用Agilent Eclipse Plus C_(18) RRHD柱(2.1 mm×50 mm,1.8μm),以乙腈-0.1%甲酸水为流动相进行梯度洗脱。质谱分析均采用电喷雾正离子模式采集。UPLC-Q-TOF-MS通过对照品比对及高分辨质谱数据解析,推测了东革阿里中32种苦木素二萜成分并解析了其裂解规律。UPLC-QQQ-MS/MS定量分析东革阿里中4种苦木素二萜成分,在考察的浓度范围内线性关系良好(r≥0.999 6),回收率为90.35%~106.4%,RSD为1.8%~3.6%。该方法快速、可靠、高效,能较全面地反映东革阿里中的苦木素二萜类成分及含量,可为深入阐明东革阿里的药效物质基础及其质量标准研究提供参考。
In this work, a sensitive and efficient method was established and validated for qualitative and quantitative analysis of major quassinoid diterpenoids constituents from the extract of Eurycoma longifolia by ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) and ultra-performance liquid chromatography coupled with a triple quadrupole mass spectrometry(UPLC-QQQ-MS/MS). The UPLC-Q-TOF-MS analysis was performed on an Agilent Eclipse Plus C_(18) RRHD(2.1 mm×100 mm,1.8 μm) column with acetonitrile and 0.1% formic acid water as mobile phase by gradient elution. The UPLC-QQQ-MS/MS analysis was performed on an Agilent Eclipse Plus C_(18) RRHD(2.1 mm×50 mm, 1.8 μm)column with acetonitrile and 0.1% formic acid water as mobile phase by gradient elution. The data was collected by electrospray ionization in positive mode. According to the contrast of the reference standards and the accurate masses of molecules, a total of 32 quassinoid diterpenoids in E. longifolia extract were identified by UPLC-Q-TOF-MS. For quantitative the linear range of 4 detected quassinoid diterpenoids were good(r≥0.999 6), and the overall recoveries ranged from 90.35% to 106.4%, with the RSD ranging from 1.8% to 3.6%. The method was accurate, reliable and efficient, and could comprehensively reflect the chemical constituents and content of E. longifolia, and could provide a reference for further elucidating its pharmacological basis and quality control.

关键词(KeyWords): 东革阿里;UPLC-Q-TOF-MS;UPLC-QQQ-MS/MS;定性分析;定量分析;苦木素二萜
Eurycoma longifolia;UPLC-Q-TOF-MS;UPLC-QQQ-MS/MS;qualitative analysis;quantitative analysis;quassinoid diterpenoids

Abstract:

Keywords:

基金项目(Foundation): 福建省属公益类科研院所基本科研专项(2017R1009-8)

作者(Author): 陈秀明;方东升;周璟明;郑孝贤;林斌;王海龙;詹清;
CHEN Xiu-ming;FANG Dong-sheng;ZHOU Jing-ming;ZHENG Xiao-xian;LIN Bin;WANG Hai-long;ZHAN Qing;Fujian Provincial Key Laboratory of Screening for Novel Microbial Products, Fujian Institute of Microbiology;

Email:

DOI: 10.19540/j.cnki.cjcmm.20200630.201

参考文献(References):

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