LC-MS/MS法测定跌打酒中9种成分及主成分分析  

Determination of 9 constituents in Die Da Jiu by LC-MS/MS and analysis of its principal component

作　　者：蓝晓庆 韦瑀龙[2,3] 陆兰娟 LAN Xiao-qing;WEI Yu-long;LU Lan-juan(Guangxi Zhuang Autonomous Region Testing Institute of Product Quality,Nanning 530001,China;Ruikang Hospital Affiliated to Guangxi University of Chinese Medicine,Nanning 530001,China;Guangxi Scientific Research Center of Traditinal Chinese Medicine,Nanning 530001,China;Guangxi Min Sheng Zhong Jian Lian Detection Co.Ltde,Nanning 530001,China)

机构地区：[1]广西产品质量检验研究院,广西南宁530001 [2]广西中医药大学附属瑞康医院,广西南宁530001 [3]广西壮瑶药工程技术研究中心,广西南宁530001 [4]广西民生中检联检测有限公司,广西南宁530001

出　　处：《实用药物与临床》2021年第1期67-71,共5页Practical Pharmacy and Clinical Remedies

基　　金：广西高校中青年教师基础能力提升项目(J16026)。

摘　　要：目的建立跌打酒中9种成分的含量测定方法,并进行主成分分析。方法采用液质联用色谱法,kinetex C 18为色谱柱,0.1%甲酸的2 mmol/L乙酸铵溶液-甲醇为流动相,梯度洗脱,流速0.35 ml/min,ESI正负离子同时采集,多反应监测测定跌打酒中马钱子碱、士的宁、三七皂苷、大黄酸、大黄酚、大黄素、大黄素甲醚、人参皂苷Rb 1、人参皂苷Rg 1的含量;测定10批样品中9个成分的含量,并采用SPSS 19.0软件进行主成分分析。结果在优化的色谱质谱条件下,9个成分的线性关系良好,平均加样回收率为94.66%~103.57%;经主成分分析,3个主成分因子的累积方差贡献率为87.106%。结论所建立的LC-MS/MS测定方法及主成分分析可为跌打酒的质量控制和评价提供参考。Objective To establish a method for determination of 9 constituents in Die Da Jiu,and to conduct principal component analysis.Methods The LC-MS/MS method was used and the chromatographic conditions were as follows:kinetex C 18(50 mm×3 mm,2.6μm)column with gradient elution of methanol-water(containing 0.1%formic acid and 2 mmol/L ammonium acetate)at a flow rate of 0.35 ml/min.Mass spectrometer conditions:A triple quadrupole mass spectrometer equipped with ESI was used in positive and negative ion modes,and MRM was performed in selected ion recording(SIR)for determination of brucine,strychnine,rhein,Chrysophanol,emodin,Emodin methyl ether,notoginsenoside R 1 in 10 samples,ginsenoside Rb 1 and ginsenoside Rg 1 in 10 samples.The determination results were evaluated by principal component analysis with SPSS 19.0.Results Under the optimized conditions,these nine constituents showed good linear relationships and the average recoveries were 94.66%~103.57%.The principal component analysis showed that the cumulative contribution rate of three main component factors was 87.106%.Conclusion The established LC-MS/MS method and principal component analysis can provide reference for the quality control and evaluation of Die Da Jiu.

关 键 词：跌打酒 液相色谱-串联质谱 马钱子 大黄 三七 主成分分析 

分 类 号：O657.63[理学—分析化学] R286.0[理学—化学]