民族药苍白秤钩风LC-MS分析与含量测定研究  

Study on LC-MS Analysis and Content Determination of Cangbaichenggoufeng[Diploclisia glaucescens(Blume)Diels]

作　　者：邓青梅 黄周艳 周楚惠 赵凤仙 李耀华[1] 陈勇[1] DENG Qingmei;HUANG Zhouyan;ZHOU Chuhui;ZHAO Fengxian;LI Yaohua;CHEN Yong(Guangxi University of Chinese Medicine,Nanning 530200,Guangxi,China)

机构地区：[1]广西中医药大学,广西南宁530200

出　　处：《辽宁中医杂志》2025年第2期136-140,I0002,共6页Liaoning Journal of Traditional Chinese Medicine

基　　金：广西一流学科建设立项课题项目(2019xk105、2018XK060);广西壮瑶药重点实验室开放课题项目(GXZYKF2019-2);广西中药药效研究重点实验室研究课题项目(19-050-39-A6);广西高校中药提取纯化与质量分析重点实验室项目(桂教科研〔2014〕6号)。

摘　　要：目的应用UPLC-Q-ExactiveHRMS技术分析苍白秤钩风药材的化学成分,并基于HPLC技术建立苍白秤钩风中木兰花碱含量测定的方法。方法UPLC-Q-Exactive HRMS技术采用ACQUITY UPLC HSS T 3色谱柱(2.1 mm×150 mm,1.8μm)分离,以正离子0.1%甲酸水(B2)-0.1%甲酸乙腈(A2),负离子5 mM甲酸铵水(B1)-乙腈(A1)为流动相进行梯度洗脱,流速0.25 mL/min,柱温40℃,采用正负离子同时采集模式,全扫描及自动触发二级质谱扫描模式,对苍白秤钩风进行化学成分分析。HPLC法使用Durashell C 18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%磷酸(16∶84,V/V),等度洗脱,流速1.0 mL/min,检测波长230 nm,柱温35℃,测定苍白秤钩风中木兰花碱的含量。结果基于UPLC-Q-ExactiveHRMS技术所得到的离子碎片进行谱库匹配,共筛选出14个匹配度较高的化合物,其中包括5个黄酮类,1个木质素,3个生物碱类,4个萜类,1个甾体类化合物。采用HPLC法对木兰花碱进行含量测定,木兰花碱在3.6364~52.728μg/mL(r=0.99962)内线性关系良好,精密度、稳定性等方法学考察均符合要求,平均加样回收率为101.4%,14批广西不同产地苍白秤钩风药材的木兰花碱含量范围为0.0250%~0.1975%。结论UPLC-Q-Exactive HRMS技术为鉴定苍白秤钩风的化学成分提供了一种快速、高效的定性分析方法;所建立的HPLC测定木兰花碱含量的方法简便、快捷、准确,为苍白秤钩风药材质量标准的建立及其药材的推广使用提供了科学依据。Objective To analyze the chemical constituents of Cangbaichenggoufeng[Diploclisia glaucescens(Blume)Diels]by using UPLC-Q-Exactive HRMS technologyand to establish a determinationmethod for magnoflorine based on high performance liquid chromatography(HPLC)method.Methods ACQUITY UPLC HSS T 3 column(2.1 mm×150 mm,1.8μm)was used,using a gradient elution method with 0.1%formic acid water(B2)-0.1%formic acid acetonitrile(A2)as the positive ion and 5 mM ammonium formate water(B1)-acetonitrile(A1)as the negative ion as the mobile phase.The flow rate was 0.25 mL/min.The column temperature was 40℃.It adopted the simultaneous acquisition mode of positive and negative ions,full scan and automatic triggering of the secondary mass spectrometry scan mode,analyzed the chemical composition of Cangbaichenggoufeng[Diploclisia glaucescens(Blume)Diels].HPLC was performed on Durashell C 18 column(4.6 mm×250 mm,5μm).The mobile phase was acetonitrile-0.1%phosphoric acid(16∶84,V/V),and the flow rate was 1.0 mL/min,the detection wavelength was 230 nm and the column temperature was 35℃.The content of magnoflorine was determined by HPLC method.Results Based on UPLC-Q-XActive HRMS technology,14 compounds with high matching degree were screened for spectral library matching of ion fragments,including 5 flavonoids,1 lignin,3 alkaloids,4 terpenesand 1 steroid compound.HPLC method was used to determine the content of magnoflorine,and the linear relationship of magnoflorine was good within 3.6364~52.728μg/mL(r=0.99962).The precision,stability and other methodological tests met the requirements,and the average recovery rate was 101.4%.The content range of magnoflorine in 14 batches ofCangbaichenggoufeng[Diploclisia glaucescens(Blume)Diels]from different origins in Guangxi was 0.0250%~0.1975%.Conclusion UPLC-Q-Exactive HRMS technology provided a rapid and efficient qualitative analytical method for the identification of the chemical components in Cangbaichenggoufeng[Diploclisia glaucescens(Blume)Diels],and the developed HPLC method was s

关 键 词：苍白秤钩风 UPLC-Q-Exactive HRMS HPLC 含量测定 

分 类 号：R284[医药卫生—中药学]