摘要
目的:采用超高效液相-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q/Exactive),建立卫矛科不同属药材中12种成分的快速定量检测方法。方法:将卫矛科药材进行粉碎后过筛,甲醇超声提取。采用UPLC^(®)HSS T3柱(2.1 mm×100 mm,1.8μm)、以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,后采用配有电喷雾离子源的四极杆/静电场轨道阱高分辨质谱在正离子模式下进行检测,内标法进行定量。结果:该方法线性较好,线性范围广,12种化学成分在0.8~2000.0 ng/ml范围内都有着良好的线性关系,相关系数(R^(2))均>0.99;样品加样回收率为97.9%~108.0%,相对标准偏差为0.1%~1.2%。结论:该法具有快速、操作简便、准确度高的优点,可用于卫矛科药材成分快速定量分析,更好的促进卫矛科药材的合理利用,扩大可使用的药材种类,为中药资源的科学开发提供一定依据。
Objective:A rapid quantitative detection method for 12 chemical constituents in different genera of Celastraceae wasestablished by ultra-high-performance liquid-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry(UHPLC-Q/Exactive).Methods:Different genera of Celastraceae are crushed,sieved,and extracted with methanol ultrasonically.UPLC^(®)HSS T3 column(2.1 mm×100 mm,1.8μm)was used for gradient elution with the mobile phase consists of 0.1%formic acid aqueous solution asthe aqueous phase and acetonitrile as the organic phase,and the detection was performed with quadrupole/electrostatic field orbitrap highresolution mass spectrometry with electrospray ion source in positive ion mode,and internal standard method is used for quantification.Results:The method had good linearity and wide linear range.The 12 chemical components all had good linear relationship in the range of 0.8~2000 ng/ml,R^(2)>0.99.The sample spiked recoveries were 97.1%~108.0%,and the relative standard deviations were 0.1%~1.2%.Conclusion:This method has the advantages of rapidness,simple operation and high accuracy.It can be used for the rapid quantitativeanalysis of the constituents of Celastraceae,which can better promote the rational use of Celastraceae expand the available classes of herbs,and provide a certain basis for scientific development of Chinese medicine resources.
作者
柳雨亭
王玉琳
周华
杨涛
LIU Yuting;WANG Yulin;ZHOU Hua;YANG Tao(Department of Cardiovascular,Shuguang Hospital Affiliated to Shanghai University of Traditional Chinese Medicine,Institute of Cardiovascular Disease of Integrated Traditional Chinese and Western Medicine,Shanghai 201203,China;Shanghai Key Clinical Laboratory of Traditional Chinese Medicine,Shanghai 201203,China)
出处
《上海中医药大学学报》
CAS
2022年第S01期246-252,263,共8页
Academic Journal of Shanghai University of Traditional Chinese Medicine
基金
上海市医学领军人才计划项目(2015年046号)
上海市中医药事业三年行动计划(〔2018-2020〕-CCCX-5001,ZY〔2018-2020〕-CCCX-2003)
上海市科委科技支撑项目(20S21901800)
上海中医药大学产业发展中心医养结合科创项目(YYKC-2021-01-49)
作者简介
柳雨亭,女,在读硕士生,主要从事中药药效物质基础与作用机制研究;通信作者:杨涛,副研究员,硕士生导师,E-mail:yangtao@shutcm.edu.cn;通信作者:周华,研究员,博士生导师,E-mail:zhouhua@shutcm.edu.cn
