3,5-二硝基苯甲酸功能化的金属有机框架CAU-10-NH-DNBA荧光检测硫化氢  

Fluorescent Detection of Hydrogen Sulfide Using Metal-organic Framework CAU-10-NH-DNBA Functionalized with 3,5-Dinitrobenzoic Acid

作　　者：龚文朋 周林楠 GONG Wenpeng;ZHOU Linnan(College of Chemistry and Chemical Engineering,Huanggang Normal University,Huanggang 438000,China)

机构地区：[1]黄冈师范学院化学化工学院,黄冈438000

出　　处：《高等学校化学学报》2024年第8期80-88,共9页Chemical Journal of Chinese Universities

基　　金：湖北本科高校省级教学改革研究项目(批准号:2023473);黄冈师范学院重大培育项目(批准号:202211104);黄冈师范学院博士基金(批准号:2042021036)资助.

摘　　要：设计合成了一种基于3,5-二硝基苯甲酸功能化的金属有机框架CAU-10-NH-DNBA荧光探针,可直接用于H_(2)S的检测.首先,以三氯化铝和5-氨基间苯二甲酸为原料,在溶剂热条件下合成了金属有机框架CAU-10-NH_(2);然后,在水溶液中,以CAU-10-NH_(2)和3,5-二硝基苯甲酸(DNBA)为原料,在偶联剂1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐(EDC)和N-羟基琥珀酰亚胺(NHS)的共同作用下,合成了CAU-10-NH-DNBA.采用红外光谱、X射线衍射谱、固体核磁共振波谱、X射线光电子能谱和扫描电子显微镜对其进行了表征.结果表明,CAU-10-NH-DNBA的激发和发射波长分别为320和412 nm;H_(2)S可使CAU-10-NH-DNBA荧光增强;并考察了pH值、时间和温度对检测效果的影响.在最佳实验条件下,CAU-10-NH-DNBA对H_(2)S的检出限为2.43μmol/L,线性范围为3.9~62.5μmol/L,具有选择性高的优点.该探针可应用于人血清样品中H_(2)S含量的检测,样品回收率为94.5%~96.1%.Fluorescent probe based on 3,5-dinitrobenzoic acid functionalized metal-organic framework CAU-10-NHDNBA was designed for the direct detection of H_(2)S.Firstly,Metal-organic framework CAU-10-NH_(2) was synthesized using AlCl3 and 5-amino-m-phthalic acid as raw materials under solvothermal conditions.Subsequently,CAU-10-NHDNBA was synthesized in an aqueous solution using CAU-10-NH_(2) and 3,5-dinitrobenzoic acid(DNBA)as raw materials under the action of coupling agents 1-(3-dimethylaminopropyl)-3-ethylcarbimide(EDC)and N-hydroxysuccinamide(NHS).The excitation and emission wavelengths of the prepared CAU-10-NH-DNBA are 320 and 412 nm,respectively.The product was characterized by infrared spectroscopy,X-ray diffraction,solid state NMR,X-ray photoelectron spectroscopy and scanning electron microscopy.The influence of pH value,time and temperature on the detection effect was explored.Under the optimal conditions,the detection limit of H_(2)S was 2.43μmol/L,and the linear range was 3.9—62.5μmol/L.The CAU-10-NH-DNBA has the advantages of high sensitivity and selectivity,and can be applied to the determination of H_(2)S in human serum samples with a recovery range of 94.5%—96.1%.

关 键 词：金属有机框架 3 5-二硝基苯甲酸 功能化 荧光检测 硫化氢 

分 类 号：O657.3[理学—分析化学] X831[理学—化学]