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引用本文:   宋青青, 张珂, 李婷, 管朋维, 龚兴成, 许霞, 李军, 屠鹏飞, 宋月林. 反相-亲水作用色谱-定制多反应监测法同步测定肉苁蓉多成分含量. 分析化学, 2020, 48(11): 1573-1582. doi:  10.19756/j.issn.0253-3820.201104 [复制]

Citation:   SONG Qing-Qing , ZHANG Ke , LI Ting , GUAN Peng-Wei , GONG Xing-Cheng , XU Xia , LI Jun , TU Peng-Fei , SONG Yue-Lin . Simultaneous Determination of Multiple Components of Cistanches Herba Based on Reversed Phase-Hydrophilic Interaction Chromatography-Tailored Multiple Reaction Monitoring. Chinese Journal of Analytical Chemistry, 2020, 48(11): 1573-1582. doi: 10.19756/j.issn.0253-3820.201104 [复制]

反相-亲水作用色谱-定制多反应监测法同步测定肉苁蓉多成分含量

通讯作者:  屠鹏飞, pengfeitu@163.com; 宋月林, syltwc2005@163.com

收稿日期: 2020-02-28

基金项目: 本文系国家重点研发计划项目(Nos.2018YFC1707300,2017YFC702400)、国家科学自然基金项目(Nos.81773875,81530097)和北京中医药大学青年科学家培育计划项目(No.BUCM-2019-QNKXJB006)资助

Simultaneous Determination of Multiple Components of Cistanches Herba Based on Reversed Phase-Hydrophilic Interaction Chromatography-Tailored Multiple Reaction Monitoring

Corresponding author:  TU Peng-Fei , pengfeitu@163.com; SONG Yue-Lin , syltwc2005@163.com

Received Date:  2020-02-28

Fund Project:  This work was supported by the National Key Research and Development Project (Nos. 2018YFC1707300, 2017YFC702400), the National Natural Science Foundation of China (Nos. 81773875, 81530097), the Young Elite Scientists Sponsorship Program by CAST (No. 2017QNRC001) and the Young Scientist Program by Beijing University of Chinese Medicine (No. BUCM-2019-QNKXJB006).

建立了反相色谱-亲水作用色谱-定制多反应监测(RPLC-HILIC-tailored MRM)方法,对肉苁蓉中极性跨度大、含量差异大的27个化学成分的含量进行同步测定。利用RPLC与HILIC的在线直接偶联实现大、中、小极性化学成分的同步色谱保留和分离。Acquity UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8 μm)用于RPLC,Xbridge Amide色谱柱(150 mm×4.6 mm,3.5 μm)用于HILIC,色谱柱间通过混合器引入稀释泵来解决色谱机制不一致的问题。泵A(0.1%甲酸-水)和泵B(乙腈)输送流动相至RPLC柱进行梯度洗脱,流速为0.15 mL/min;泵C(0.1%甲酸-水)和泵D(乙腈)以1.0 mL/min的流速输送流动相至混合器,改变RPLC柱洗脱液的组成,促进极性大的化学成分在HILIC柱中的保留。通过灵活调节在线碰撞能,提高微量成分的质谱响应,抑制常量成分的质谱响应,形成定制多反应监测模式。最终同步测定36批肉苁蓉中27个化学成分,包括氨基酸类、有机酸类、糖类、苯乙醇苷类、环烯醚萜类、木质素类等类型。方法检出限为0.0032~160 μg/g,定量限为0.032~320 μg/g,线性相关系数大于0.9929,加标回收率为74.7%~125.1%,相对标准偏差(RSD)为1.6%~13.7%。本方法线性范围宽、准确度高、适用性广,为肉苁蓉及其它中药化学成分的深入定量分析提供了有效手段。

关键词:   反相色谱-亲水作用色谱, 定制多反应监测模式, 极性跨度, 含量跨度, 肉苁蓉
Key words:   Reversed phase-hydrophilic interaction chromatography, Tailored multiple reaction monitoring, Polarity span, Content span, Cistanches herba
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反相-亲水作用色谱-定制多反应监测法同步测定肉苁蓉多成分含量

宋青青, 张珂, 李婷, 管朋维, 龚兴成, 许霞, 李军, 屠鹏飞, 宋月林

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