黄草乌栽培品UPLC-MS/MS多指标含量测定及化学计量学分析  

UPLC-MS/MS multi-index content determination and chemometric analysis of the cultivated Radix Aconitum Vilmoriniani

作　　者：陈威 程子丹 李国栋 马晓霞 CHEN Wei;CHENG Zidan;LI Guodong;MA Xiaoxia(Yunnan University of Chinese Medicine,Kunming 650500,Yunnan,China)

机构地区：[1]云南中医药大学,云南昆明650500

出　　处：《云南大学学报(自然科学版)》2025年第2期365-372,共8页Journal of Yunnan University(Natural Sciences Edition)

基　　金：国家自然科学基金(82160746);云南省“万人计划”青年拔尖人才专项(YNWR-QNBJ-2019-011)。

摘　　要：建立超高效液相色谱-三重四级杆质谱多重反应监测(multiple reaction monitoring,MRM)定量分析方法,检测黄草乌中生物碱含量,为黄草乌的质量控制提供参考.色谱柱:ACQUITY UPLC?BEH C_(18)(ϕ2.1 mm×50 mm,1.7μm);流动相:乙腈(A)-0.1%甲酸水溶液(B)梯度洗脱;测定18批黄草乌中塔拉萨敏、滇乌碱、黄草乌碱甲等9个生物碱成分的含量,并结合化学计量法对测定结果进行分析.测定的9个成分在相应质量浓度范围内与峰面积的线性关系良好(R^(2)>0.9980),平均加样回收率为96.74%~101.2%,RSD为0.65%~1.9%.测定结果表明黄草乌中9个成分含量差异较大,无明显的地域性差别.根据聚类分析、主成分分析和正交偏最小二乘法-判别分析的结果发现18份黄草乌栽培品基本可以分两类,其中塔拉萨敏、黄草乌碱甲、滇乌碱、膝乌宁碱丙、南乌碱乙为主要差异成分.建立了UPLC-MS/MS同时测定黄草乌栽培品中9个生物碱成分含量的方法,该方法分析时间短、专属性强、灵敏度高,可为不同产地的黄草乌质量评价提供参考.A multiple indexes quantitative analysis method using ultra performance liquid chromatographyunited triple quadrupole mass spectrometry in multiple reaction monitoring(MRM)for determination of alkaloidcontent in Radix Aconitum Vilmoriniani was established.The research provide a reference for the quality controlof Radix Aconitum Vilmoriniani.Chromatography columns:ACQUITY YPLC®BEH C_(18)(ϕ2.1 mm×50 mm,1.7μm).Mobile Phases:acetonitrile(A)-0.1%formic acid aqueous solution(B),gradient elution.The contents oftalatisamine,yunaconitine,vilmorrianine A and other six deterpenoid alkaloids in 18 batches of cultivated RadixAconitum Vilmoriniani were determined by UPLC-MS/MS and evaluated combining with chemometric methods.Good linearity(R^(2)>0.9980)was observed for the contents of nine ingredients with respect to their peak areasmeasured in the corresponding concentration ranges.The average spiked recovery rate were 96.74%-101.2%withthe RSD of 0.65%-1.9%.The determination results showed that the contents of nine components in RadixAconitum Vilmoriniani varied largely,but there were no significant geographical differences.According to theresults of HCA,PCA and OPLS-DA,18 batches of cultivated Radix Aconitum Vilmoriniani were found to bebasically divided into two categories,in which talatismine,vilmorrianine A,yunaconitine,geniculatine C andaustroconitine B were the main differential components.The method was developed for the simultaneousdetermination of the contents of nine alkaloid components in cultivated Radix Aconitum Vilmoriniani by UPLC-MS/MS.The method have advantage of high specificity and sensitivity with short analysis time,and can provide areference for the quality evaluation of Radix Aconitum Vilmoriniani from different origins.

关 键 词：黄草乌 超高效液相色谱串联质谱法 含量测定 化学计量学 

分 类 号：O657.63[理学—分析化学] R284.1[理学—化学]