氮和硼双掺杂碳点的合成及其用于苦味酸检测  

Synthesis of Nitrogen and Boron Co-doped Carbon Dots for Picric Acid Detection

作　　者：王英特[1] 杨玉洁 段蓉 张媛媛 王云霞 WANG Yingte;YANG Yujie;DUAN Rong;ZHANG Yuanyuan;WANG Yunxia(School of Chemistry and Chemical Engineering,Shanxi University,Taiyuan 030006,China;Shanxi Lishanyuan Liquor Co.,Ltd,Taiyuan 030063.China)

机构地区：[1]山西大学化学化工学院,山西太原030006 [2]山西绿膳源酒业有限公司,山西太原030063

出　　处：《山西大学学报（自然科学版）》2022年第2期431-440,共10页Journal of Shanxi University(Natural Science Edition)

基　　金：2020小店区-山西大学产学研合作项目;山西省自然科学基金(201801D121074)。

摘　　要：以柠檬酸为碳源,乙二胺和四苯基硼钠分别作为氮和硼掺杂剂,通过水热法合成了发蓝色荧光的N,B双掺杂碳量子点(N,B-CDs)。所合成的N,B-CDs的量子产率高达75.6%,与我们之前以苦杏仁酸为碳源和乙二胺氮源合成的N-CDs碳点(量子产率为41.4%)相比有明显提高。通过TEM、FT-IR、XRD、XPS、Raman、UV-vis和FL等表征方法对N,B-CDs的表面形貌,官能团和光学性质等进行了表征。结果表明N,B-CDs为平均直径为3.6 nm的球形结构,最佳荧光发射波长和激发波长分别为442 nm和342 nm。并且该N,B-CDs表面具有丰富的亲水基团,使得所合成的碳点具有良好的水溶性。基于苦味酸(PA)与N,B-CDs之间可能存在的荧光共振能量转移机制和内滤效应,N,B-CDs的荧光能被PA有效猝灭,可用于PA的检测。在最佳实验条件下,N,B-CDs的荧光强度与PA的浓度在0.1μmol·L^(-1)~24.7μmol·L^(-1)之间呈现良好的线性关系,相应的检出限为0.019μmol·L^(-1)。并且该方法已成功用于实际水样中PA含量的检测,相应的回收率为95.80%~103.10%。To improve sensitivity and selectivity of picric acid(PA) detection by carbon dots(CDs),the quantum yield(QY) of the synthesized CDs was increased via co-doping ethylenediamine and sodium tetraphenylboron as nitrogen(N) and boron(B) dopants to modify the CDs surfaces.The QY of the obtained N,B-CDs was higher up to 75.6% which was obviously improved by comparison to our previous reported N-CDs synthesized by mandelic acid as carbon sources and ethylenediamine as nitrogen sources.The surface morphology and optical properties of N,B-CDs were investigated.The consequences revealed that N,B-CDs were spherical structure,and the average diameter was 3.6 nm.The optimal emission and excitation wavelength of the synthesized N,B-CDs were442 nm and 342 nm,accompanied by bright blue fluorescence.The fourier transform infrared spectroscopy showed that there were abundant hydrophilic groups on N,B-CDs surface,which made N,B-CDs have good water solubility.A strategy for selectively and sensitively detecting PA by the synthesized N,B-CDs was based on PA quenching the FL intensity of CDs via a possible fluorescence resonance energy transfer mechanism and inner filter effect.Under the optimum conditions of experiment,the N,B-CDs fluorescence intensity showed a great linear correlation with the PA concentration between 0.1 μmol·L^(-1)to 24.7 μmol·L^(-1),and the limit of detection was 0.019 μmol·L^(-1)(S/N=3).In addition,the N,B-CDs were employed to detect PA of real water samples and satisfactory results were obtained.The recoveries ranged from 95.80% to 103.10%.

关 键 词：苦味酸 柠檬酸 双掺杂碳点 乙二胺 四苯硼酸钠 荧光猝灭 

分 类 号：O621[理学—有机化学]