超高效液相色谱-飞行时间质谱联用分析柏芩清火颗粒中的化学成分(Ⅰ)

目的分析柏芩清火颗粒中的化学成分。方法采用超高效液相色谱-飞行时间质谱联用(UPLC-TOF-MS)方法。色谱柱为ACQUITY UPLC BEH C18柱(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸溶液(A)-0.1%甲酸乙腈溶液(B),流速为0.35 mL.min-1。ESI-MS检测采用负离子模式。通过与方中主要的单味药对比判断色谱峰的来源药材,继而通过与来源药材化学成分进行精确分子量的对比鉴定化合物。结果对柏芩清火颗粒中来源于熟地、黄芩等5味药材中的洋地黄叶苷C,苦奥诺苷A1、B1,芹糖甘草苷,异麦角甾苷,黄芩苷,牡丹皮苷C、B,汉黄芩素,甘草皂苷G2、H2,黄芪甲苷,黄芪皂苷Ⅰ、Ⅱ,乙酰黄芪皂苷等23个化合物进行了鉴定,体现了复方的多成分组成特性。结论 UPLC的高分离度结合TOF-MS的高分辨质谱为中药复方化学成分的研究提供了一种快速有效的方法。

Chemical constituents of Baiqin Qinghuo Keli by UPLC-TOF-MS(I)

Objective To qualitatively analyze the chemical constituents of Baiqin Qinghuo Keli.Methods UPLC-TOF-MS was employed for analysis.Chromatograph was carried out on ACQUITY UPLC BEH C18 column（2.1 mm × 100 mm,1.7 μm） with 0.1% formic acid in water（A） and 0.1% formic acid in acetonitrile（B） at 0.35 mL·min-1 as the mobile phase.ESI-MS data were acquired in a negative mode.Major constituents in the preparation were characterized by matching their accurate mass with that of the constituents of source herbs.Results A total of 23 compounds derived from 5 herbs were indentified,i.e.,purpureaside C,jionoside A1 and B1,liquiritin apioside,isoacteoside,baicalin,mudanpioside C and B,wogonin,licoricesaponin G2 and H2,astragaloside Ⅳ,astragaloside Ⅰ,Ⅱ and a cetylastragaloside Ⅰ,reflecting the multiple constituents composition of Chinese medicinal formulae effectively.Conclusion High resolution of UPLC coupled with accurate mass obtained from TOF-MS provide a rapid and efficient method for chemical analysis of Chinese traditional formulae.