锆基金属有机框架键合开管柱的制备及其毛细管电色谱应用  

Preparation of the bonded open tubular column based on Zr-organic framework and its application in capillary electrochromatography

作　　者：初美凤 赵明[1,2,3] 高立娣 初红涛[1,2,3] 曲欣然 徐栖笛[1] 陈默 孟繁舒 秦世丽 靳凤龙 CHU Meifeng;ZHAO Ming;GAO Lidi;CHU Hongtao;QU Xinran;XU Qidi;CHEN Mo;MENG Fanshu;QIN Shili;JIN Fenglong(College of Chemistry and Chemical Engineering,Qiqihar University,Qiqihar 161000,China;Technology Innovation Center of Industrial Hemp for State Market Regulation,Qiqihar 161000,China;Heilongjiang Industrial Hemp Processing Technology Innovation Center,Qiqihar 161000,China;Qiqihar Inspection and Testing Center,Qiqihar Administration for Market Regulation,Qiqihar 161000,China)

机构地区：[1]齐齐哈尔大学化学与化学工程学院,齐齐哈尔161000 [2]国家市场监管技术创新中心(工业大麻),齐齐哈尔161000 [3]黑龙江省工业大麻加工技术创新中心,齐齐哈尔161000 [4]齐齐哈尔市场监督管理局齐齐哈尔检验检测中心,齐齐哈尔161000

出　　处：《分析试验室》2024年第11期1578-1585,共8页Chinese Journal of Analysis Laboratory

基　　金：黑龙江省教育厅基本科研专项(145209503)项目资助。

摘　　要：采用原位聚合法,以Zr Cl_(4)为金属源,四[4-(4’-羧基苯基)苯基]乙烯为有机配体,制备了毛细管电色谱键合开管柱。所制备固定相具有较大的比表面积和较高的结晶度,且在毛细管柱内分布均匀、与柱壁紧密连接。以硫脲为中性标记物,考察了日内平均柱效、日间平均柱效及柱间的平均柱效,3种平均柱效在2.4×10^(4)~2.7×10^(4) plates/m范围内相对标准偏差(RSD)小于3.1%。所制备的毛细管电色谱键合开管柱实现了对5种苯系物、6种磺胺类抗生素、3种碱性氨基酸的快速有效分离,说明其具有良好的稳定性、重现性及分离性能。基于此,建立了工业大麻籽中3种碱性氨基酸的毛细管电色谱定性、定量分析方法。结果表明,在2.0~100.0μg/m L范围内,峰面积与浓度呈良好的线性关系,精氨酸、赖氨酸和组氨酸的检出限(LOD)分别为0.6,2.5和1.3μg/m L,定量限(LOQ)分别为2.0,8.3和4.3μg/m L,样品加标回收率大于87.4%,RSD小于4.5%。Using Zr Cl_(4) as the metal source and 4[4-(4'-carboxyphenyl) phenyl]ethylene as the organic ligand,the capillary electrochromatographic bonded open tubular column was prepared by in situ polymerization method.The prepared stationary phase not only had large specific surface area and high crystallinity but also was evenly distributed in the capillary column and closely connected with the column internal wall.The intra-day,intra-day and inter-column average column efficiencies were investigated by using thiourea as neutral marker.The results showed that the average column efficiencies ranged from 2.4×10^(4) to 2.7×10^(4) plates/m,and the relative standard deviations (RSDs) were less than 3.1%.The separation of 5 benzene series,6 sulfonamide antibiotics and 3 basic amino acids was achieved fast and effectively,indicating that the prepared open tubular column displayed good stability,reproducibility and separation performance.Meanwhile,the qualitative and quantitative analysis method of three basic amino acids in industrial Cannabis seeds was established using the open tubular column as a separation channel.The results showed that there were good linear relationships between the peak areas and the concentrations in the range of 2.0-100.0μg/m L.The limits of detection (LODs) of arginine,lysine and histidine were 0.6,2.5 and 1.3μg/m L,and the limits of quantification (LOQs) were 2.0,8.3 and 4.3μg/m L,respectively,the recoveries were more than 87.4%,and the RSDs were less than 4.5%.

关 键 词：锆基金属有机骨架 键合开管柱 毛细管电色谱 工业大麻籽 

分 类 号：O657.3[理学—分析化学]