气相色谱-质谱法测定烷基酚含量中酚类衍生条件优化  

Optimization of Derivatization Conditions of Phenols in Determination of Alkylphenols by Gas Chromatography-Mass Spectrometry

作　　者：周同娜 尹海亮[2] ZHOU Tong-na;YIN Hai-liang(Environmental Protection Agency of Dongying,Dongying 257091,China;Academy of Science&Technology,China University of Petroleum,Dongying 257061,China)

机构地区：[1]山东省东营生态环境监测中心,东营257091 [2]中国石油大学(华东)科学技术研究院,东营257061

出　　处：《当代化工》2022年第5期1245-1248,共4页Contemporary Chemical Industry

基　　金：生态环境部国家环境保护标准制修订管理项目,水质双酚A和烷基酚的测定气相色谱-质谱法(项目编号:No.2014-31)。

摘　　要：气相色谱-质谱法测定烷基酚含量时衍生化处理是关键步骤,通过详尽考察影响9种短链烷基酚化合物(4-特丁基酚、4-正丁基酚、4-正戊基酚、4正己基酚、4-特辛基酚、4-正庚基酚、壬基酚、4-正辛基酚和4-正壬基酚)衍生反应的相关因素,包括衍生试剂种类、衍生试剂用量、衍生时间、衍生温度、衍生介质等,获得了该系列化合物衍生反应的最优条件,衍生试剂选择BSTFA(99∶1),衍生试剂用量为100μL,衍生温度为25℃(室温),衍生时间为1h,衍生用介质为二氯甲烷。在该条件下,9种短链烷基酚化合物均能衍生完全。Derivatization is the key step in the determination of alkylphenols by gas chromatography-mass spectrometry. The related factors affecting the derivatization of nine short chain alkylphenol compounds(4-tert-butyl phenol, 4-n-butyl phenol, 4-n-pentyl phenol, 4-hexyl phenol, 4-tert-octyl phenol, 4-heptyl phenol, nonylphenol,4-n-octyl phenol and 4-octyl phenol) were studied, including the type of derivatization reagent, the amount of derivatization reagent, the time, the temperature and the medium of derivatization. The optimum conditions for derivatization of these compounds were obtained. The derivatization reagent was BSTFA(99∶1), the derivatization reagent amount was 100 μL, the derivatization temperature was 25 ℃, the derivatization time was 1 h, and the derivatization medium was dichloromethane. Under these conditions, all the nine short chain alkylphenols can be derived completely.

关 键 词：气相色谱-质谱法 烷基酚 衍生化反应 最优条件 

分 类 号：X833[环境科学与工程—环境工程]