摘要
以蔗糖为碳源,磷酸二氢铵为氮与磷源,通过一步水热法制备了一种耐酸型氮、磷掺杂碳量子点(ART-N,P-CQDs)作荧光探针,利用透射电镜(TEM)、傅里叶红外光谱(FT-IR)、纳米粒度分析仪、X-射线光电子能谱(XPS)、紫外分光光度计和荧光分光光度计对ART-N,P-CQDs的结构及其光学性质进行表征分析。结果显示,ART-N,P-CQDs为平均粒径1.7 nm的球形结构,其表面含有丰富的羟基、羧基、胺基、磷酸酯基等丰富的含氮、磷、氧的官能团,具有激发独立性的蓝色荧光,荧光量子产率为4.7%。鉴于Fe(Ⅲ)对ART-N,P-CQDs具有荧光猝灭效应,且为了准确检测Fe(Ⅲ),需将其置于酸性环境以防止三价铁水解。从而构建了一种能在酸性环境下检测微量Fe(Ⅲ)的新方法。该方法线性方程为F_(0)/F=0.00364C(Fe^(3+))+0.9901(R^(2)=0.9942),检出限为1.49μmol/L,线性范围为10~100μmol/L,能量转移猝灭和静态猝灭过程是致使ART-N,P-CQDs荧光猝灭的原因。ART-N,P-CQDs在一定酸性环境、离子强度及干扰离子共存的条件下检测体系仍具有良好的荧光稳定性,将该方法应用于补铁药品中微量铁的测定,其加标回收率为94.59%~99.53%,结果令人满意。该方法操作简便,可用于市面上补铁药片中铁含量的检测,具有一定的应用前景。
Using sucrose as carbon source and ammonium dihydrogen phosphate as nitrogen and phosphorus sources,acid-resistance type nitrogen and phosphorus doped carbon quantum dots(ART-N,P-CQDs)were synthesized by a one-step hydrothermal method and applied as fluorescent probes.The structure and optical properties of ART-N,P-CQDs were characterized by transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR),nanoparticle size analyzer,X-ray photoelectron spectroscopy(XPS),UV-visible absorption spectrum and fluorescence spectrophotometer.The results showed that ART-N,P-CQDs had a spherical structure with an average particle size of 1.7 nm,and their surfaces were rich in functional groups such as hydroxyl,carboxyl,amine,phosphate containing nitrogen,phosphorus and oxygen atoms.The quantum dots exhibits bright blue fluorescence with excitation independence and a fluorescence quantum yield of 4.7%.Considering the fluorescence quenching effect of Fe(Ⅲ)and the need for accurate detection in acidic environments to prevent hydrolysis,a new method was developed for detecting trace amounts of Fe(Ⅲ)under acidic conditions.The linear relationship was given by the equation:F_(0)/F=0.00364C(Fe^(3+))+0.9901(R^(2)=0.9942),with a limit of detection of 1.49μmol/L and a linear range of 10~100μmol/L.The fluorescence quenching mechanism was attributed to energy transfer quenching and static quenching.The detection system maintained good fluorescence stability under acidic conditions,varying ionic strength,and coexistence of interfering ions.The method was successfully applied to the determination of trace iron in commercial iron supplementation,yielding spiked recoveries of 94.59%to 99.53%with satisfactory results.Owing to its operational simplicity and reliability,the proposed method demonstrates promising potential for iron quantification in commercially iron supplements.
作者
吴楚仪
吕枭
李华辉
张荩之
吴煜琳
黎天云
赵丹华
WU Chu-yi;LV Xiao;LI Hua-hui;ZHANG Jin-zhi;WU Yu-lin;LI Tian-yun;ZHAO Dan-hua(College of Chemistry and Materials Science;Research Center for Environmental Materials and Resource Utilization,Guangdong University of Education,Guangzhou 510303,China)
出处
《化学试剂》
2025年第8期38-44,共7页
Chemical Reagents
基金
广东第二师范学院污水处理与监测科研创新团队资助项目(2024 KYCXTD016)
大学生创新实验项目(202414278005)
广东省级本科质量工程教育教学改革项目(粤高教函〔2021〕29号-416)
广东省教育厅重点领域专项项目(2022ZDZX4037,2024ZDZX2087)
广州市基础与应用基础研究项目(202201011099)。
关键词
耐酸性
氮、磷掺杂的碳量子点
激发独立性
Fe(Ⅲ)检测
荧光探针
acid resistance
nitrogen and phosphorus doped carbon quantum dots
excitation independence
detection of Fe(Ⅲ)
fluorescence probe
