基于HPLC-MS的救必应多指标成分的含量测定  

Multi-compound determination of Llicis Rotundae Cortex base on HPLC-MS

作　　者：刘振杰[1] 高红伟 孙雪萍 谭小明 许琼明 覃喜军 LIU Zhen-jie;GAO Hong-wei;SUN Xue-ping;TAN Xiao-ming;XU Qiong-ming;QIN Xi-jun(Guangxi University of Chinese Medicine,Nanning 530299,China)

机构地区：[1]广西中医药大学,南宁530299

出　　处：《药物分析杂志》2021年第11期1868-1874,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金(81860711,81860270);广西自然科学基金(2018GXNSFBA281034);广西科技基地和人才专项(桂科AD19245124);广西中医药大学2017年引进博士科研启动基金项目(2017BS035,2017BS031);中国-东盟传统医药发展研究中心开放课题(0501801727,0501801726)。

摘　　要：目的:建立救必应的高效液相色谱串联质谱(HPLC-MS)多指标成分的含量测定方法,为救必应质量控制提供科学依据。方法:采用Waters CORTECS C_(18)(2.1 mm×100 mm,2.7μm)色谱柱,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.4 mL·min^(-1);采用电喷雾离子源负离子选择离子监测模式(SIR),锥孔电压15 V,毛细管电压0.8 kV条件下扫描,建立咖啡酸、紫丁香苷、长梗冬青苷、毛冬青皂苷B_(2)、毛冬青皂苷甲、冬青素A、铁冬青酸7个指标成分的含量测定方法。结果:咖啡酸、紫丁香苷、长梗冬青苷、毛冬青皂苷B_(2)、毛冬青皂苷甲、冬青素A、铁冬青酸在相应的浓度范围内与峰面积呈良好的线性关系,精密度、稳定性、重复性的RSD值均小于2.0%,平均加样回收率为95.2%~104.1%,11批救必应样品中上述7个成分含量依次为0~0.8074、0~15.81、37.26~52.35、0~3.668、0~5.966、0~0.7397、3.24~28.33 mg·mL^(-1)。结论:本方法建立的检测方法简便可靠,重现性好,专属性强,可为救必应的质量研究提供相关参考依据。Objective:To develop a new content determination method for multi-component determination of Llicis Rotundae Cortex based on HPLC-MS,and provide a scientific basis for its quality standard.Methods:Waters CORTECS C_(18) column(2.1 mm×100 mm,2.7μm)was used to analyze the components with mobile phase of acetonitrile-0.1%formic acid aqueous solution in gradient elution mode at a flow rate of 0.4 mL·min^(-1).Syringin,caffeic acid,pedunculoside,ilexsaponin B_(2),ilexsaponin A,rotundic acid and ilexgenin A were determined by selective ion monitoring in negative ion mode with 15 V cone voltage and 0.8 kV capillary voltage.Results:Syringin,caffeic acid,pedunculoside,ilexsaponin B_(2),ilexsaponin A,rotundic acid and ilexgenin A in Llicis Rotundae Cortex had good linear relationship,the RSD values of precision,stability and repeatability wereunder 2.0%,and the sample recoveries were 95.2%-104.1%.The contents of seven components in Llicis Rotundae Cortex from different areas were between 0-0.8074,0-15.81,37.26-52.35,0-3.668,0-5.966,0-0.7397 and 3.24-28.33 mg·mL^(-1).Conclusion:The method was established for content determination of seven components in Llicis Rotundae Cortex.It could provide reference for the quality evaluation of Llicis Rotundae Cortex.

关 键 词：救必应 紫丁香苷 长梗冬青苷 铁冬青酸 液相色谱-质谱联用 单四极杆质谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]