目的 建立超快速液相色谱-三重四级杆/线性离子阱质谱法(UFLC-QTRAP-MS/MS)同时测定不同产地竹节参药材中皂苷、氨基酸及核苷类共33种成分含量的方法。方法 采用XBridge C18(4.6 mm×100 mm,3.5 μm),以0.1%甲酸水-0.1%甲酸乙腈为流动相,梯度洗脱,流速0.8 mL·min-1,柱温30 ℃,多反应监测离子扫描模式(MRM)测定。结果 33种成分在一定浓度内均呈现良好的线性关系,相关系数均大于0.999 0;精密度、重复性和稳定性良好;平均加样回收率为96.95%~101.8%,RSD均小于5%。结论 所建立的方法准确、可靠,可为竹节参药材内在质量的综合评价和全面控制提供新的方法参考。
Abstract
OBJECTIVE To develop a method for the determination of saponins, amino acids and nucleosides in Panacis Japonici Rhizoma from different habitats by UFLC-QTRAP-MS/MS. METHODS The chromatographic separation was performed on an XBridge C18 coulumn(4.6 mm×100 mm,3.5 μm) at 30 ℃ with gradient elution of 0.1% formic acid solution-0.1% formic acid acetonitrile, and the flow rate was 0.8 mL·min-1, using multiple-reaction monitoring(MRM) mode. RESULTS The 33 constituents showed good linearity(r>0.999 0) in the range of the tested concentrations; the precision, repeatability and stability were good; the average recovery rates were between 96.95% and 101.8%, and the relative standard deviations were less than 5%. CONCLUSION The established method is accurate and reliable, which can be used as a reference for the quality evaluation and control of Panacis Japonici Rhizoma.
关键词
超快速液相色谱-三重四级杆/线性离子阱质谱法 /
竹节参 /
皂苷 /
氨基酸 /
核苷
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Key words
UFLC-QTRAP-MS/MS /
Panacis Japonici Rhizoma /
saponin /
amino acid /
nucleoside
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中图分类号：
R917
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脚注
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基金
江苏高校优势学科建设工程项目资助(YSXK-2014);江苏高校品牌专业建设工程项目资助(PPZY2015A070)
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