柱前荧光衍生化法检测降尘样品中的不饱和醛  

Detection of Unsaturated Aldehydes in Dust Samples Based on a Pre-Column Derivatization Strategy

作　　者：黄露杰 徐静 汪耀[2] 吕敏 崔玉洁 何振宇[2] 林亚维 HUANG Lujie;XU Jing;WANG Yao;L Min;CUI Yujie;HE Zhenyu;LIN Yawei(Department of Chemistry,School of Chemistry,Chemical Engineering&Life Sciences,Wuhan University of Technology,Wuhan 430070;Wuhan Center for Disease Control&Prevention,Wuhan 430060)

机构地区：[1]武汉理工大学化学化工与生命科学学院,湖北武汉430070 [2]武汉市疾病预防控制中心,湖北武汉430060

出　　处：《分析科学学报》2024年第2期153-158,共6页Journal of Analytical Science

基　　金：湖北省卫健委预防专项重大项目(No.WJ2019H303);武汉预防医学科研专项(No.WY19M01)。

摘　　要：本研究发展了一种柱前荧光衍生化方法,实现了重要环境污染物不饱和醛类化合物的高灵敏度、高选择性分析。该方法使用4-丁基羟氨-7-羟基香豆素(HAHC)作为荧光衍生试剂,结合高效液相色谱-荧光检测法(HPLC-FLD)实现了6种二烯醛的定性、定量分析。在实际样品分析中成功从积尘样品中检测出(E,E)-2,4-庚二烯醛、(E,E)-2,4-辛二烯醛、(E,E)-2,4-十一烷二烯醛。这种柱前衍生化法具有动态范围宽(2~2500nmol/L)、灵敏高(检出限为0.2nmol/L)、精密度好(日内相对标准偏差为2.17%~3.33%,日间相对标准偏差为2.28%~5.04%)等优点,且无需固相萃取等复杂前处理步骤,为痕量醛类污染物检测提供了有效手段。Unsaturated aldehydes are a kind of important environmental pollutants.In this study,a pre-column derivatization strategy was developed combined with a liquid chromatography-fluorescence detection method(HPLC-FLD)using 4-butylhydroxylamine-7-hydroxycoumarin(HAHC)as a fluorescent derivatization reagent.After the optimization of the derivatization conditions,a precolumn derivatization method was developed and applied for the analysis of six unsaturated aldehydes with LODs as low as 0.2 nmol/L.In the real sample analysis,(E,E)-2,4-Heptadienal,(E,E)-2,4-Octadienal,(E,E)-2,4-Undecadienal were detected with concentrations in the range of 12.70-136.87μmol/L.The method has a wide dynamic range(2-2500 nmol/L)and good precision(intraday RSDs 2.17%-3.33%,interday RSDs 2.28%-5.04%)without complex pretreatment steps,providing a method for the monitoring of unsaturated aldehyde pollutants in various fields.

关 键 词：硝酮化衍生法 不饱和醛 高效液相色谱-荧光检测法 4-羟氨基丁基-7-甲氧基-香豆素 

分 类 号：O657.72[理学—分析化学]