目的 建立超高效液相色谱-串联四级杆/线性离子阱质谱(QTRAP UPLC-MS/MS)同时测定乌药中生物碱(去甲异波尔定、波尔定碱)、内酯类(乌药内酯、乌药醚内酯、异乌药内酯、乌药醇、去氢木香内酯)和黄酮类(儿茶素、表儿茶素、异槲皮苷)成分的方法,比较乌药不同部位中各成分的含量差异。方法 样品经甲醇超声辅助提取,稀释后采用ACQUITY UPLCRHSS T3(2.1 mm×100 mm,1.8 μm),保护柱:Cartridge Guarde Colume E Inertsil ODS-SP(4.0 mm×10 mm,5 μm);以水(含0.1%甲酸,A相)-乙腈(B相)为流动相;梯度洗脱,柱温35 ℃,流速0.2 mL·min-1,进样量5 μL。采用电喷雾离子源(ESI),多反应离子监测(MRM)扫描方式进行检测。结果 10种目标化合物在一定浓度范围内均呈良好的线性关系,相关系数大于0.991 6,精密度、重复性和稳定性良好;加样回收率在99.13%~103.07%,RSD值均小于5%。结论 所建立的方法简便、灵敏度高、重现性好,可用于乌药中多元功效物质的同时测定,为乌药药材内在质量的综合评价和综合利用提供新的方法参考。
Abstract
OBJECTIVE To develop a comprehensive analytical method based on QTRAP UPLC-MS/MS for simultaneous determination of three kinds of components in Lindera aggregate (Sims) Kosterm(L. aggregate). METHODS The samples were extracted by methanol aided with ultrasound, diluted and then separated on a ACQUITY UPLCRHSS T3(2.1 mm×100 mm,1.8 μm)column, with Cartridge Guarde Colume E Inertsil ODS-SP(4.0 mm×10 mm,5 μm) as protection column. The mobile phase was composed of acetonitrile-water (0.1% acetic acid) and eluted at a flow rate of 0.2 mL·min-1. The target compounds were analyzed by multiple reactions monitoring (MRM) mode. RESULTS The assay for the ten components had good linearity, the linearity of the detected components was greater than 0.991 6 and the limits of detection were all satisfying. The average spiked recoveries for the compounds were between 99.13% and 103.07%, and the relative standard deviations were less than 5%. CONCLUSION The established method is simple, sensitive, accurate, and suitable for determination of ten components in L. aggregate, which can provide a reliable and effective technique for the quality control of L. aggregate.
关键词
乌药 /
超高效液相色谱-串联四级杆/线性离子阱质谱 /
生物碱 /
内酯 /
黄酮
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Key words
Lindera aggregate (Sims) Kosterm /
QTRAP UPLC-MS/MS /
alkaloid /
lactone /
flavonoid
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中图分类号：
R284
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脚注
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基金
浙江省中医药优秀青年人才基金项目资助(2019ZQ041);宁波市自然科学基金项目(2018A610434,2019A610414);浙江中医药大学省重点建设高校优势特色学科(中药学)开放基金资助(ZYAOX2018025,ZYAOX2018028);浙江省大学生科技创新活动计划暨新苗人才计划项目资助(2019R458003,2020R424003)
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