超高效液相色谱-高分辨质谱法同时测定类叶牡丹中9种三萜皂苷类成分  

Rapid simultaneous determination of nine triterpene saponins constituents of Caulophyllum robustum by UPLC-FT/MS

作　　者：梁军[1] 夏永刚[1] 郭信东 王天龙 匡海学[1] LIANG Jun XIA Yong-gang GUO Xin-dong WANG Tian-long KUANG Hai-xue(Key Laboratory of Chinese Materia Medica, Ministry of Education, Heilongjiang Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharrnacodynamic Material Bases, Heilongjiang University of Chinese Medicine, Harbin 150040, China)

机构地区：[1]黑龙江中医药大学教育部北药基础与应用研究重点实验室黑龙江省中药及天然药物药效物质基础研究重点实验室,黑龙江哈尔滨150040

出　　处：《中草药》2017年第20期4323-4327,共5页Chinese Traditional and Herbal Drugs

基　　金：国家科技部国家重大新药创制专项(2013ZX09102019);黑龙江省自然科学基金面上项目(H2017063);黑龙江省普通本科高等学校青年创新人才项目(2016209);黑龙江省博士后基金(LBH-Q13158;LBH-Z10019;LBH-Z15209);教育部重点实验室--北药基础与应用研究开放课题基金资助(2015bs06)

摘　　要：目的建立超高效液相色谱-高分辨质谱法(UPLC-FT/MS)同时测定类叶牡丹Cauorlhyllum robustum中9种三萜皂苷类成分的方法。方法采用正离子模式;色谱柱:ACE Excel 3 C_(18)(100 mm×2.1 mm,3.0μm);保护柱:ACE Excel 3C_(18)(12.5 mm×4.6 mm,3.0μm);流动相为0.1%甲酸水(A)-乙腈(B)溶液,梯度洗脱,体积流量0.40 m L/min,柱温35℃。结果定量分析的类叶牡丹中三萜皂苷类成分在考察的浓度范围内呈良好的线性关系(r>0.996);加样回收率和RSD分别在98.49%~107.03%和1.00%~3.33%。结论本研究建立的同时测定类叶牡丹中9种三萜皂苷类成分的UPLC-FT/MS定量分析方法灵敏度高、分辨率高、质量稳定并且简便、准确,可为综合评价类叶牡丹的质量提供参考。Objective To establish a rapid simultaneously determination of nine triterpene saponins of Cauorlhyllum robustum by UPLC-FT/MS. Methods UPLC-MS/MS assay in positive ion mode was performed on a ACE Excel 3 C18（100 mm × 2.1 mm, 3.0 μm） with the mobile phase consisting of 0.1% formic acid aqueous（A） and 0.1% formic acid acetonitrile（B） in gradient elution at a flow rate of 0.40 mL/min and the column temperature was set at 35 ℃. Results Satisfactory linearity was achieved with wide linear range and fine linear relationship（r 0.996 3）, the recoveries were ranged from 98.49% to 107.03% with the RSD ranging from 1.00% to 3.33%. Conclusion It is the first report about simultaneous analysis of nine triterpene saponins of Cauorlhyllum robustum by UPLC-FT/MS method, which affords highly sensitive, resolution, simple, accurate, and speedy efficient method for quality control of Cauorlhyllum robustum.

关 键 词：类叶牡丹 超高效液相色谱-高分辨质谱法 三萜皂苷 质量控制 葳严仙皂苷H 葳严仙皂苷G 葳严仙皂苷B 葳严仙皂苷C 

分 类 号：R286.2[医药卫生—中药学]