中国中药杂志

2019, v.44(06) 1208-1215

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丹参和紫丹参脂溶性成分的UPLC及LC-MS/MS分析
Analysis of lipophilic components of Salvia miltiorrhiza roots and S. yunnanensis roots by UPLC and LC-MS/MS

张立国;胡甜甜;张芳芳;栾绍嵘;李巍;邓海星;兰竹慧;罗晓芳;吴中相;Leslaw Mleczko;
ZHANG Li-guo;HU Tian-tian;ZHANG Fang-fang;LUAN Shao-rong;LI Wei;DENG Hai-xing;LAN Zhu-hui;LUO Xiao-fang;WU Zhong-xiang;Leslaw Mleczko;School of Chemistry & Molecular Engineering,East China University of Science and Technology;Sichuan Dian Hong Pharmaceutical Development Co.,Ltd.;Bayer China Co.,Ltd.;Bayer Germany Co.,Ltd.;

摘要(Abstract):

采用超高效液相色谱及液-质联用技术分析16批丹参和18批紫丹参脂溶性成分指纹图谱并进行比较。液相条件:Thermo Accucore C_(18)色谱柱(2.1 mm×100 mm,2.6μm);流动相为0.026%磷酸水(A)-乙腈(B),梯度洗脱;流速0.4 m L·min~(-1);检测波长270 nm;进样量2μL;柱温25℃。液质条件:Q Exactive Orbitrap LC-MS/MS,流动相为0.1%的甲酸水(A),0.1%甲酸和乙腈(B),梯度洗脱,采用电喷雾离子源,正离子模式下采集数据。丹参脂溶性成分有10个共有峰,16批不同产地丹参与丹参对照图谱的相似度大于0.942、平均相似度为0.973;紫丹参脂溶性成分有12个共有峰,18批紫丹参与紫丹参对照图谱的相似度大于0.937、平均相似度为0.976;丹参对照图谱和紫丹参对照图谱间的相似度为0.900。紫丹参中有3个丹参中没有的脂溶性成分,其中一个结构为α-拉帕醌;丹参中有1个紫丹参中没有的脂溶性成分丹参新酮;2种药材含有丹参酮Ⅱ_A、去甲丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、去甲丹参酮在内的8个共同脂溶性成分,其中紫丹参的丹参酮Ⅱ_A(P<0.05)、丹参酮Ⅰ(P<0.05)、去甲丹参酮Ⅰ(P<0.05)、隐丹参酮(P<0.01)、二氢丹参酮Ⅰ(P<0.01)的含量显著低于丹参。丹参、紫丹参中脂溶性成分的种类及含量存在显著差异。
Fingerprints of lipophilic components in the roots of Salvia miltiorrhiza and S.yunnanensis were analyzed by UPLC-DADand UPLC coupled with mass spectroscopy to evaluate the differences and similarities of the lipophilic components in the two kinds of herbs.The UPLC analysis of 18 batches of S.miltiorrhiza and 16 batches of S.yunnanensis was performed on a 25℃Thermo Accucore C_(18)column(2.1 mm×100 mm,2.6μm)by Shimadzu LC-20AD;mobile phase was 0.026%phosphoric acid(A)-acetonitrile(B)with gradient elution;flow rate was 0.4 m L·min~(-1);detection wavelength was set at 270 nm;injection volume was 2μL.The molecular structures of the lipophilic components were analyzed on a 25℃Thermo Accucore C_(18)column(2.1 mm×100 mm,2.6μm)by Thermo U3000 UPLC Q Exactive Orbitrap LC-MS/MS with a mobile phaseconsisting of 0.1%formic acid water(A)and 0.1%formic acidacetonitrile(B).The mass spectrometry was acquired in positive modes using ESI.There are 10 common peaks in the lipophilic components of S.miltiorrhiza.The similarity between the 16 batches of S.miltiorrhiza and their own reference spectra was greater than 0.942,and the average similarity was 0.973.There are 12 common peaks in the lipophilic components of S.yunnanensis.The similarity between the 18 batches of S.yunnanensis and their own reference spectra was greater than 0.937,and the average similarity was 0.976.The similarity between the reference chromatograms of S.miltiorrhiza and S.yunnanensis was only 0.900.There are three lipophilic components in S.yunnanensis,which are not found in S.miltiorrhiza,and one of which isα-lapachone.There is a lipophilic component in S.miltiorrhiza not found in S.yunnanensis,which may be miltirone.The two herbs contain 8 common lipophilic components including dihydrotanshinoneⅠ,cryptotanshinone,tanshinoneⅠ,tanshinoneⅡ_A,nortanshinone in which the content of tanshinoneⅡ_A,dihydrotanshinoneⅠand cryptotanshinone of S.yunnanensisis significantly lower than that of S.miltiorrhiza(P<0.01),and the contents of tanshinoneⅠand nortanshinone are significantly lower than that of S.miltiorrhiza too(P<0.05).There are significant differences in the types and contents of lipophilic components between the roots of S.miltiorrhiza and S.yunnanensis,and the similarity between the fingerprints of interspecies is much lower than that between the same species.Therefore,the roots of S.miltiorrhiza and S.yunnanensis are two kinds of herbs which are quite different in chemical compounds and compositions.

关键词(KeyWords): 丹参;紫丹参;脂溶性成分指纹图谱;超高效液相色谱;液质联用
Salvia miltiorrhiza;S.yunnanensis;fingerprints of lipophilic components;UPLC;LC-MS-MS

Abstract:

Keywords:

基金项目(Foundation): 国家“重大新药创制”科技重大专项(2018ZX09721003-009-002)

作者(Author): 张立国;胡甜甜;张芳芳;栾绍嵘;李巍;邓海星;兰竹慧;罗晓芳;吴中相;Leslaw Mleczko;
ZHANG Li-guo;HU Tian-tian;ZHANG Fang-fang;LUAN Shao-rong;LI Wei;DENG Hai-xing;LAN Zhu-hui;LUO Xiao-fang;WU Zhong-xiang;Leslaw Mleczko;School of Chemistry & Molecular Engineering,East China University of Science and Technology;Sichuan Dian Hong Pharmaceutical Development Co.,Ltd.;Bayer China Co.,Ltd.;Bayer Germany Co.,Ltd.;

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DOI: 10.19540/j.cnki.cjcmm.20181226.020

参考文献(References):

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