固相萃取结合高效液相色谱-三重四极杆质谱快速分离检测益气养血口服液中人参皂苷的新方法  

Rapid Separation and Detection of Ginsenosides in Yiqiyangxue Oral Liquid Using High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry Combined with Solid-phase Extraction

作　　者：吴冬雪 刘淑莹 陈思键[1] 赵幻希 修洋 王淑敏 WU Dong-xue;LIU Shu-ying;CHEN Si-jian;ZHAO Huan-xi;XIU Yang;WANG Shu-min(Jilin Ginseng Academy,Changchun University of Chinese Medicine,Changchun 130117,China;Changchun Institute of Applied Chemistry,Chinese Academy of Sciences,Changchun 130022,China;College of Pharmacy,Changchun University of Chinese Medicine,Changchun 130117,China)

机构地区：[1]长春中医药大学吉林省人参科学研究院,吉林长春130117 [2]中国科学院长春应用化学研究所,吉林长春130022 [3]长春中医药大学药学院,吉林长春130117

出　　处：《分析测试学报》2020年第7期867-873,共7页Journal of Instrumental Analysis

基　　金：国家自然科学基金(21475012);吉林省教育厅“十三五”科学技术项目(JJKH20181274KJ)。

摘　　要：以无机多孔材料作为固相萃取吸附剂,结合高效液相色谱-三重四极杆质谱(HPLC-QqQ/MS)建立了一种快速分离检测中药复方益气养血口服液中人参皂苷的新方法。考察了SAPO-34、SAPO-11、ZSM-5、Y型分子筛、SBA-15、多壁碳纳米管(MWCNTs)6种无机多孔材料对4种主要人参皂苷Re、Rg1、Rb1、Ro的吸附活性。在优化条件下,MWCNTs的分离效果最好,可在2 min内分别达到吸附和脱附平衡,吸附率和脱附回收率分别达98.6%和96.8%以上。方法的检出限为0.01~0.05μg/mL,平均回收率为90.5%~99.7%,相对标准偏差为2.2%~4.9%。益气养血口服液中4种人参皂苷含量的分析结果显示,建立的方法对口服液中除皂苷外的其他成分吸附作用不明显,可以有效降低基质干扰并准确分析微量的人参皂苷。该方法在快速检测人参皂苷方面具有潜在的应用价值。A novel high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-QqQ/MS),based on solid-phase extraction(SPE)with inorganic porous materials as the adsorbents,was developed for the rapid separation and detection of ginsenosides in Yiqiyangxue oral liquid,a Chinese medicine compound.The adsorption activities of SAPO-34,SAPO-11,ZSM-5,zeolite Y,SBA-15 and multi-walled carbon nanotubes(MWCNTs)on ginsenoside Re,Rg1,Rb1 and Ro were investigated.Under the optimized conditions,MWCNTs exhibited the best separation performance as they could reach an adsorption and desorption equilibrium towards ginsenosides within two minutes,respectively.The adsorption rates and desorption recoveries were higher than 98.6%and 96.8%,respectively.The limits of detection were in the range of 0.01-0.05μg/mL,and the average recoveries were between 90.5%and 99.7%with relative standard deviations of 2.2%-4.9%.Moreover,the developed method was validated to be accurate and sensitive enough to detect and quantify trace amount of ginsenosides.Finally,the new method was successfully used for the separation and detection of the 4 ginsenosides in Yiqiyangxue oral liquid.Results revealed that the method has no obvious adsorption effect on the components other than ginsenosides,reducing the matrix interference and increasing the accuracy of quantification.Hence,HPLC-QqQ/MS combined with the proposed MWCNTs-based SPE has a great application potential in the rapid detection of ginsenosides.

关 键 词：无机多孔材料 人参皂苷 固相萃取 高效液相色谱-三重四极杆质谱(HPLC-QqQ/MS) 

分 类 号：O657.63[理学—分析化学] R914.1[理学—化学]