中国中药杂志

2019, v.44(11) 2283-2291

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基于UPLC-Q-TOF-MS/MS技术的夹竹桃寄主及其桑寄生强心苷成分相关性研究
Correlation study on chemical constitutes of cardiac glycosides in Taxillus chinensis and its Nerium indicum host by UPLC-Q-TOF-MS/MS

刘人源;黄蜚颖;郭敏;陆海琳;朱开昕;覃文慧;覃展敏;李永华;苏本伟;
LIU Ren-yuan;HUANG Fei-ying;GUO Min;LU Hai-lin;ZHU Kai-xin;QIN Wen-hui;QIN Zhan-min;LI Yong-hua;SU Ben-wei;Guangxi University of Chinese Medicine;Qinzhou Institute of Traditional Chinese Medicine;Wuzhou Yuanjiangxiangshui Sangjisheng Bio-Technique Co., Ltd.;

摘要(Abstract):

建立超高效液相色谱-飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS)的夹竹桃寄主及其桑寄生强心苷成分鉴定方法,评价寄主对桑寄生药材质量影响。采集夹竹桃寄主及其桑寄生样品,用桑树寄主及其桑寄生为对照样品,样品用70%乙醇超声提取。使用ACQUITY UPLC HSS T3 C_(18)色谱柱(2.1 mm×100 mm,1.8μm),以流动相0.1%甲酸水-乙腈梯度洗脱,流速0.6 mL·min(-1),进样量0.5μL,柱温40℃。根据正、负离子模式质谱数据及元素组成分析,结合强心苷对照品和相关文献,对夹竹桃寄主及其桑寄生强心苷成分进行鉴定,并分析它们之间的相关性。共鉴定出强心苷化合物29个,其中夹竹桃寄主强心苷28个,夹竹桃寄主的桑寄生强心苷5个,桑树寄主及其桑寄生没有强心苷。采用液质联用技术能快速、准确、全面地鉴定寄主夹竹桃及其桑寄生强心苷成分,结果为评价寄主对桑寄生药材质量影响提供参考依据。
To build up an identification method on cardiac glycosides in Taxillus chinensis and its Nerium indicum host, and evaluate the influence on medicine quality from host to T. chinensis, ultra-performance liquid chromatography coupled with quadrupole-time-of-flight tandem mass-mass spectrometry(UPLC-Q-TOF-MS/MS)was applied. The samples of T. chinensis(harvested from N. indicum)and its N. indicum host were collected in field. The samples of T. chinensis(harvested from Morus alba)and its M. alba host was taken as control substance. All samples were extracted by ultrasonic extraction in 70% ethanol. Chromatographic separation was performed on an ACQUITY UPLC HSS T3 C_(18)(2.1 mm×100 mm,1.8 μm)column at 40 ℃. Gradient elution was applied, and the mobile phase was consisted of 0.1% formic acid water and acetonitrile. The 0.5 μL of sample solution was injected and the flow rate of the mobile phase was kept at 0.6 mL·min(-1),进样量0.5μL,柱温40℃。根据正、负离子模式质谱数据及元素组成分析,结合强心苷对照品和相关文献,对夹竹桃寄主及其桑寄生强心苷成分进行鉴定,并分析它们之间的相关性。共鉴定出强心苷化合物29个,其中夹竹桃寄主强心苷28个,夹竹桃寄主的桑寄生强心苷5个,桑树寄主及其桑寄生没有强心苷。采用液质联用技术能快速、准确、全面地鉴定寄主夹竹桃及其桑寄生强心苷成分,结果为评价寄主对桑寄生药材质量影响提供参考依据。
To build up an identification method on cardiac glycosides in Taxillus chinensis and its Nerium indicum host, and evaluate the influence on medicine quality from host to T. chinensis, ultra-performance liquid chromatography coupled with quadrupole-time-of-flight tandem mass-mass spectrometry(UPLC-Q-TOF-MS/MS)was applied. The samples of T. chinensis(harvested from N. indicum)and its N. indicum host were collected in field. The samples of T. chinensis(harvested from Morus alba)and its M. alba host was taken as control substance. All samples were extracted by ultrasonic extraction in 70% ethanol. Chromatographic separation was performed on an ACQUITY UPLC HSS T3 C_(18)(2.1 mm×100 mm,1.8 μm)column at 40 ℃. Gradient elution was applied, and the mobile phase was consisted of 0.1% formic acid water and acetonitrile. The 0.5 μL of sample solution was injected and the flow rate of the mobile phase was kept at 0.6 mL·min(-1) in each run. It was done to identify cardiac glycosides and explore the chemical composition correlation in T. chinensis and its N. indicum host by analyzing positive and negative ion mode mass spectrometry data, elemental composition, cardiac glycoside reference substance and searching related literatures. A total of 29 cardiac glycosides were identified, 28 of it belonged to N. indicum host, 5 belonged to T. chinensis(harvested from N. indicum host), none of cardiac glycoside was identified in T. chinensis(harvested from M. alba host). The result could provide a reference in evaluating the influence in T. chinensis medicine quality from host. It was rapid, accurate, and comprehensive to identify cardiac glycosides in T. chinensis and its N. indicum host by UPLC-Q-TOF-MS/MS.

关键词(KeyWords): 夹竹桃;桑寄生;强心苷;UPLC-Q-TOF-MS/MS
Nerium indicum;Taxillus chinensis;cardiac glycoside;UPLC-Q-TOF-MS/MS

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81660669,81173537);; 广西自然科学基金项目(2017GXNSFAA198316);; 广西一流学科建设项目重点课题(2018XK027);; 广西中医药大学中药学优势学科建设专项(ZYXZ2015002),广西中医药大学中药提取与质量分析重点实验室开放课题(J1700206);; 广西卫生厅中医药科技专项(GZZY13-39);; 广西自治区研究生科研创新项目(YCSW2017172)

作者(Authors): 刘人源;黄蜚颖;郭敏;陆海琳;朱开昕;覃文慧;覃展敏;李永华;苏本伟;
LIU Ren-yuan;HUANG Fei-ying;GUO Min;LU Hai-lin;ZHU Kai-xin;QIN Wen-hui;QIN Zhan-min;LI Yong-hua;SU Ben-wei;Guangxi University of Chinese Medicine;Qinzhou Institute of Traditional Chinese Medicine;Wuzhou Yuanjiangxiangshui Sangjisheng Bio-Technique Co., Ltd.;

DOI: 10.19540/j.cnki.cjcmm.20190415.202

参考文献(References):

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