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)同时测定鸡血藤不同产地及商品药材中黄烷醇、异黄酮、黄酮醇、二氢黄酮、二氢黄酮醇、查耳酮、紫檀烷、花色素和酚酸类共22种活性成分含量的方法;根据22种目标成分的含量,用主成分分析对不同产地的鸡血藤药材进行综合评价。方法 采用XBridge C18柱(4.6 mm×100 mm, 3.5 μm),以0.3%甲酸水-甲醇为流动相,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;根据22种目标成分的含量,用主成分分析(PCA)对所检测的31个批次鸡血藤药材进行综合评价。结果 22种目标成分的浓度与峰面积的线性关系良好(r>0.999 0);平均加样回收率为97.95%~103.1%,RSD均小于5%。结论 所建立的方法准确、可靠,可用于鸡血藤中多元功效物质或指标成分的同时测定,为鸡血藤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 simultaneous determination of flavanols, isoflavones, flavonols, dihydroflavones, flavanonols, chalcones, pterocarpan, anthocyanidins and phenolic acids in Spatholobi Caulis from different habitats and commercial herbs by UFLC-QTRAP-MS/MS. Principal component analysis (PCA) was applied to comprehensively analyze and evaluate the results of multiple active constituents. METHODS The chromatographic separation was performed on an XBridge C18 column (4.6 mm×100 mm, 3.5 μm) at 30 ℃ with gradient elution by 0.3% formic acid aqueous solution-methanol, and the flow rate was 0.8 mL·min-1, using multiple-reaction monitoring (MRM) mode. Principal component analysis (PCA) was performed to evaluate 31 samples according to the contents of 22 constituents. RESULTS The 22 target components showed good linearity (r>0.999 0) in the range of the tested concentrations. The average recovery rates of the 22 components were from 97.46% to 103.6% with relative standard deviations less than 5%. CONCLUSION The developed method is accurate and reliable, and could be used for simultaneous determination of multi-functional substances or index components in Spatholobi Caulis, which could provide a reference for the comprehensive evaluation and quality control of Spatholobi Caulis.
关键词
超快速液相色谱-三重四级杆/线性离子阱质谱法 /
鸡血藤 /
多元活性成分 /
主成分分析 /
黄酮 /
酚酸
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Key words
UFLC-QTRAP-MS/MS /
Spatholobi Caulis /
multiple bioactive constituent /
principal component analysis /
flavonoid /
phenolic acid
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中图分类号：
R284
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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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