目的 建立超高效液相色谱-三重四级杆/线性离子阱质谱(UPLC-QTRAP-MS/MS)同时测定苍耳草中酚酸、蒽醌及黄酮类18种活性成分的方法,并对其多元活性成分的动态积累进行分析与评价。方法 采用Agilent ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5 μm),以甲醇-0.2%甲酸水溶液为流动相,梯度洗脱,负离子多反应监测(MRM)模式测定;用灰色关联度分析对多元活性成分进行综合评价。结果 18种活性成分的浓度与峰面积的线性关系良好(r>0.999 4);平均加样回收率为96.96%~102.55%,RSD值均小于3%。苍耳草中各成分的积累动态不一,7月中、下旬综合质量较好。结论 为揭示苍耳草中多元活性成分的动态积累规律及确定其药材的适宜采收期提供基础资料,同时为苍耳草药材内在质量的综合评价提供新的方法参考。
Abstract
OBJECTIVE To develop a method for the determination of phenolic acids, anthraquinones, and flavonoids in Xanthii Herba at different harvest time by UPLC-QTRAP-MS/MS and analyze the dynamic accumulation of multiple active components in Xanthii Herba. METHODS Chromatographic separation was conducted on an Agilent ZORBAX SB-C18 (4.6 mm×250 mm, 5 μm) column with gradient elution using methanol and 0.2% formic acid as mobile phases. MS analysis was carried out using electrospray ionization in negative MRM mode. Grey related degree was used for the comprehensive evaluation. RESULTS The calibration curves for the 18 components showed good linearity (r>0.999 4) in the range of the tested concentrations. The average recoveries of the 18 components were from 96.96% to 102.55% with relative standard deviations (RSDs) less than 3%. There were differences in the contents of 18 components in Xanthii Herba at different harvest periods. Xanthii Herba had high quality in late July and mid-July. CONCLUSION This study reveals the rule of the dynamic accumulation of 18 components in Xanthii Herba and provides information for the suitable harvest time.
关键词
苍耳草 /
超高效液相色谱-三重四级杆/线性离子阱质谱 /
酚酸 /
蒽醌 /
黄酮 /
动态积累 /
综合评价
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Key words
Xanthii Herba /
UPLC-QTRAP-MS/MS /
phenolic acid /
anthraquinones /
flavonoid /
dynamic accumulation /
comprehensive evaluation
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中图分类号：
R284
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脚注
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基金
盐城市医学科技发展计划资助项目(YK2014051);江苏高校优势学科建设工程资助项目(YSXK-2014);江苏高校品牌专业建设工程资助项目(PPZY2015A070)
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