PNTU探针-荧光猝灭法测定Hg^(2+)的含量  

Determination of Hg by Fluorescence Quenching with PNTU Probe

作　　者：刘丹 陈安银 向文军[1] 颜爽 杨雄 LIU Dan;CHEN Anyin;XIANG Wenjun;YAN Shuang;YANG Xiong(School of Chemistry and Chemical Engineering,Sichuan University of Arts and Science,Dazhou 635000,China;Key Laboratory of Exploitation and Study of Distinctive Plants in Education Department of Sichuan Province,Sichuan University of Arts and Science,Dazhou 635000,China)

机构地区：[1]四川文理学院化学化工学院,达州635000 [2]四川文理学院“特色植物开发研究”四川省高校重点实验室,达州635000

出　　处：《理化检验（化学分册）》2021年第8期682-687,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：四川省科技厅资助项目(2018JY0299);四川省达州市科技局项目(20YYJC0001);四川省特色植物开发与研究重点实验室项目(TSZW2009);四川文理学院水处理研究专项(2018SCL005Y)。

摘　　要：制备了一种硫脲分子PNTU探针,基于其对Hg^(2+)的专一性比色识别,建立了荧光猝灭法测定Hg^(2+)含量的方法。在4-溴-1,8-萘酐的乙醇溶液中,逐滴加入2 mL 80%(质量分数)水合肼溶液,反应完成后,经抽滤,乙醇、水洗涤后干燥,再加入10 mL吡咯烷,在氮气保护下继续反应,得到红褐色固体。将其溶于15 mL乙腈中,室温搅拌下滴加1 mL异硫氰酸苯酯,反应完成后,经减压浓缩、水洗得到PNTU探针。将PNTU探针溶液与体积比为8∶2的乙腈-4-羟乙基哌嗪乙磺酸缓冲液的混合液混匀,然后加入含Hg^(2+)的样品溶液,采用荧光猝灭法测定体系的荧光强度。结果显示:当加入Hg^(2+)时,体系的荧光强度明显降低,溶液颜色由黄色变成橙红色;干扰试验表明PNTU探针在有其他金属离子存在的情况下仍可检测出Hg^(2+);Hg^(2+)浓度在20.0μmol·L-1以内与其对应体系的荧光强度降低值呈线性关系,检出限(3S/N)为1.8 nmol·L-1;对实际水样进行3个浓度水平的加标回收试验,Hg^(2+)的回收率为99.6%~104%,测定值的相对标准偏差(n=5)为0.85%~2.6%。基于PNTU探针制备了Hg^(2+)的检测试纸,可方便快捷地检测样品中是否存在Hg^(2+)。Based on specific colorimetric recognition of Hg^(2+)with PNTU probe,a method for the determination of Hg^(2+)by fluorescence quenching was established.In the ethanol solution of 4-bromo-1,8-naphthalene anhydride,2 mL of 80%(mass fraction)hydrazine hydrate solution was added dropwise.After filtering,washing with ethanol and water and drying,pyrrolithane of 10 mL was added.Then reaction was running under the protection of nitrogen to give reddish-brown solid.The reddish-brown solid was dissolved in 15 mL of acetonitrile,and 1 mL of phenyl isothiocyanate was added by stirring at room temperature.After the reaction was completed,the PNTU probe was obtained after vacuum concentration and washing with water.PNTU probe solution was evenly mixed with a mixture of acetonitrile-4-hydroxyethyl piperazine ethanesulfonic acid buffer solution at volume ratio of 8∶2,then Hg^(2+)sample soution was added,and fluorescence intensity of the system was measured by fluorescence quenching.The results showed that the fluorescence intensity of PNTU system decreased obviously when Hg^(2+)was added,following color of the solution changed from yellow to orange-red,and the PNTU probe could detect Hg^(2+)in the presence of other metal ions.Linear relationship between concentration of Hg^(2+)and magnitude of decrease in fluorescence intensity of the system was kept within 20.0μmol·L-1,with detection limit(3 S/N)of 1.8 nmol·L-1.Recovery test was made by standard addition method on actual water samples at 3 concentration levels,giving results in the range of 99.6%-104%,and RSDs(n=5)of the determined values ranged from 0.85%to 2.6%.Detection strips based on PNTU probe were prepared,which could easily and quickly detect whether Hg^(2+)exists in the sample.

关 键 词：荧光猝灭法 Hg2+ 比色识别 PNTU探针 检测试纸 

分 类 号：O657.3[理学—分析化学]