藏药独一味中30种化学成分的UPLC-ESI-TOFMS分析鉴定

Analysis of Thirty Chemical Constituents in Tibetan Medicine Lamiophlomis rotata by UPLC-ESI-TOF MS

目的:建立快速高效的方法,对藏药独一味的化学成分进行有效的鉴定,为该药材质量监督提供技术支持。方法:采用超高效液相-电喷雾-飞行时间质谱(UPLC-ESI-TOF MS)联用技术,色谱分离用ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm),流动相组成比例分别为0.05%甲酸水和乙腈,梯度洗脱,流速0.3 m L·min-1,进样量1μL;质谱定性采用飞行时间质谱,正离子模式扫描。结果:在优化的液质联用条件下,通过电喷雾-飞行时间质谱鉴定出独一味30个成分,分别为(1)phlomiol;(2)lamalbid;(3)phlorigidoside C;(4)胡麻属苷;(5)山栀苷甲酯;(6)5-羟基马钱苷;(7)vanillyl-O-β-D-葡萄糖苷;(8)绿原酸;(9)6-O-乙酰山栀苷甲酯;(10)cistanoside E;(11)7,8-dehydropenstemoside;(12)chlorotuberoside;(13)7-epi-loganin;(14)7-dehydroxy-2-zaluzioside;(15)马钱苷;(16)连翘酯苷B;(17)8-O-乙酰山栀苷甲酯;(18)芦丁;(19)木犀草苷;(20)毛蕊花糖苷;(21)木犀草素-7-O-β-D-呋喃芹糖基(1→6)-O-β-D-吡喃葡萄糖苷;(22)salviifoside A;(23)8-epi-7-deoxyloganin;(24)异类叶升麻苷;(25)芹菜素-7-O-β-D-葡萄糖苷;(26)6β-n-butoxy-7,8-dehydropenstemonoside;(27)芹菜素;(28)6-O-syringyl-barlerin;(29)木犀草素;(30)槲皮素。结论:通过UPLC-ESI-TOF MS联用技术,阐明了独一味的化学成分,为独一味及其制剂的质量控制和监管提供了科学依据;同时,为其他藏药的化学成分快速分析提供参考。

Objective： To find out a rapid and efficient method to analyze effectively the chemical constituents in Tibetan medicine Lamiophlomis rotata and to provide technical support for the quality supervision of the medicinal materials. Methods： UPLC-ESI-TOF MS method was used and an ACQUITY UPLC HSS T3（2.1 mm×100 mm, 1.8 μm） column was used for chromatographic seperation. The mobile phase consisted of water containing 0.05% formic acid and acetonitrile. The flow rate was 0.3 mL·min^-1 and injection volume was 1 μL in gradient elution. TOF MS was applied for qualitative analysis under positive ion mode. Results： 30 chemical constituents in Lamiophlomis rotata were identified under optimized LC-MS conditions, including phlomiol, lamalbid, phlorigidoside C, sesamoside, shanzhiside methyl ester, 5-hydroxy-loganin, vanillyl-O-β-Dglucopyranoside, chlorogenic acid, 6-O-acetyl shanzhiside methyl ester, cistanoside E, 7,8-dehydropenstemoside, chlorotuberoside, 7-epi-loganin, 7-dehydroxy-2-zaluzioside, loganin, forsythoside B, 8-O-acetyl shanzhiside methyl ester, rutin, luteoloside, acteoside, luteolin-7-O-β-D-apiofuranosy（1→6）-O-β-D-glucopyranoside, salviifoside A, 8-epi-7-deoxyloganin, isoacteoside, apigenin-7-O-β-D-glucopyranoside, 6β-n-butoxy-7,8-dehydropenstemonoside, apigenin, 6-O-syringyl-barlerin, luteolin, and quercetin. Conclusion： The chemical constituents in Lamiophlomis rotate were elucidated by UPLC-ESI-TOF MS. These results set up a scientific basis for the quality control and supervision of Lamiophlomis rotata and its preparations and provide references for the rapid analysis of chemical constituents in other Tibetan medicines.