环境样品中邻苯二甲酸酯的荧光分析条件优化  

OPTIMIZATION OF FLUORESCENCE CONDITIONS OF PHTHALIC ACID ESTERSIN ENVIRONMENTAL SAMPLES

作　　者：李冰 李玉双 魏建兵 王皓 吴尚遇 瞿维 侯永侠 宋雪英 LI Bing;LI Yu-shuang;WEI Jian-bing;WANG Hao;WU Shang-yu;QU Wei;HOU Yong-xia;SONG Xue-ying(Key Laboratory of Regional Environment and EcoRemediation of Ministry of Education,Environmental College,Shenyang University,Shenyang 110044,China)

机构地区：[1]沈阳大学环境学院区域污染环境生态修复教育部重点实验室,沈阳110044

出　　处：《环境工程》2018年第10期145-149,155,共6页Environmental Engineering

基　　金：国家自然科学基金(21307084;21377139;41771200);沈阳市科技局项目(17183900);沈阳大学大学生创新创业训练计划项目(201711035082)

摘　　要：以邻苯二甲酸正二丁酯(DnBP)作为邻苯二甲酸酯(PAEs)的模式物,采用浓硫酸增效反应增强其荧光强度,建立了一种间接测定PAEs总量的荧光分析方法并对其荧光分析条件进行优化。荧光光谱优化结果表明:最佳激发波长(λ_(ex))为218 nm,发射波长(λ_(em))为363 nm,最佳单色器宽度为5 nm,光电倍增管电压为700 V;DnBP与浓硫酸反应最适条件为硫酸浓度80%(体积分数),硫酸溶液用量为8 mL,反应时间为240 min,荧光强度在3 h内保持稳定;DnBP浓度在8.98×10^(-8)～3.59×10^(-6) mol/L范围内,其荧光强度与浓度呈良好的线性关系,方法检出限为2.95×10^(-8) mol/L,平行样品RSD为5.6%,土壤样品和水样中DnBP的回收率分别达到95%～120%和90%～115%,能够满足环境样品的分析要求。该方法操作简单、分析速度快、灵敏度高,适用于环境样品中PAEs总量的测定。An indirect determination fluorescence analysis method of total Phthalic Acid Esters（PAEs） determination was established, DnBP was taken as a kind of model substance of PAEs,through the synergistic response of concentrated sulfuric acid to enhance the fluorescence intensity,and then the fluorescence analysis conditions were optimized.The optimization results of fluorescence spectra showed that, the best excitation wavelength（ λ（ex）） was 218 nm, emission wavelength（ λ（em）） was 363 nm,the best monochromator width was 5 nm, and the photomultiplier tube voltage was 700 V;the optimum reaction conditions were as follows： the sulfuric acid concentration was 80% and the volume was 8 mL, the reaction time was 240 min, the fluorescence intensity remained stabely within 3 h; in the range of 8.98×10（-8）—3.59×10（-6） mol/L, there was a good linear relationship between the fluorescence intensity and the DnBP concentration, the detection limit was 2.95×10（-8） mol/L, and the RSD of parallel samples was 5.6%.The recovery of DnBP in soil samples and water samples was respectively in the range of 95%—120% and 90%—115%, it could meet the requirement of environmental samples analysis. The method was simple, rapid and sensitive, and suitable for the determination of total PAEs in environmental samples.

关 键 词：环境样品 邻苯二甲酸酯 荧光法 

分 类 号：X830[环境科学与工程—环境工程]