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
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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 C_(18)(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 m L/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.
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 C_(18)(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 m L/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.
引文
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[7]沙东旭,张满来.HPLC-ELSD测定三七药材及其制剂中三七皂苷R1、人参皂苷Rg1及Rb1的含量[J].中国中药杂志,2005,30(2):112-114.
[8]应弘梅,戚中杰,郭达伟,等.HPLC-ELSD测定细梗香草皂苷B与皂苷C的含量[J].中国药学杂志,2011,46(9):704-706.
[2]李国玉.类叶牡丹抗风湿有效部位的化学成分研究[D].哈尔滨:黑龙江中医药大学,2006.
[3]李国玉,徐娜,刘晓燕,等.类叶牡丹化学成分的研究[J].中草药,2015,46(10):1431-1436.
[4]张艳海.类叶牡丹皂苷类成分及其含量测定方法研究[D].哈尔滨:黑龙江中医药大学,2006.
[5]胡静,张铁军,许浚.RP-HPLC法测定三七总皂苷中3种皂苷[J].中草药,2006,37(2):218-219.
[6]陈碧莲,祝明,郭增喜,等.反相高效液相色谱法测定三七药材5种皂苷含量[J].医药导报,2010,29(11):1485-1486.
[7]沙东旭,张满来.HPLC-ELSD测定三七药材及其制剂中三七皂苷R1、人参皂苷Rg1及Rb1的含量[J].中国中药杂志,2005,30(2):112-114.
[8]应弘梅,戚中杰,郭达伟,等.HPLC-ELSD测定细梗香草皂苷B与皂苷C的含量[J].中国药学杂志,2011,46(9):704-706.