中空纤维顶空液相微萃取-气相色谱法测定胶黏剂中正己烷  

Determination of n-hexane in adhesive with hollow fiber-supported headspace liquid phase microextraction / gas chromatography

作　　者：苗佩佩 丁健桦[1] 张席席 李建强[1] 林海禄[1] 黄国林[1] 

机构地区：[1]东华理工大学化学生物与材料科学学院,南昌330013

出　　处：《分析试验室》2014年第11期1296-1300,共5页Chinese Journal of Analysis Laboratory

基　　金：江西省科技计划项目(20133BBG70105)资助

摘　　要：建立了以中空纤维顶空液相微萃取（HF-HS-LPME）为样品前处理技术,结合气相色谱法测定胶黏剂中正己烷含量的方法。通过对萃取剂的选择、温度、时间、搅拌速率、盐效应等参数的优化,确定了最佳实验条件：以邻二甲苯作为有机萃取剂,萃取温度为80℃,萃取时间为45 min,搅拌速率为700 r/min,Na Cl加入量为4 mol/L。萃取后,取0.5μL接收相进行气相色谱分析。正己烷含量的标准曲线在0.0138-1.38 g/L范围内线性关系良好,相关系数为0.9995,相对标准偏差（RSD）为2.6%,方法的检出限（LOD）为89.2μg/L（经LPM E后LOD则可达5.2μg/L）。研究还发现,正己烷初始质量浓度在3.46-138 mg/L范围内时,富集倍数随正己烷初始浓度的增大呈对数型降低,这为LPM E的理论研究提供了新的论据。方法应用于胶黏剂样品分析,平均加标回收率为92.3%-96.2%,RSD为3.6%-4.7%。A novel method for the determination of n-hexane chromatography coupled with hollow fiber-supported headspaee liquid in adhesive was established using gas phase microextration （HF-HS-LPME） as a technique for sample preparation. By optimizing control parameters, such as the selection of extraction agent, temperature, time, stirring rate and salt effect, the optimum conditions were determined as follows： o-xylene was used as an extractant, the extraction temperature was 80 ℃, the extraction time was 45 min, the stirring rate was 700 r/min and the NaCl concentration in sample solutions was 4 mol/L. After extraction, 0. 5 μL of acceptor phase was introduced to gas chromatography for analysis. The results showed that： n-hexane had good linear relation within 0. 0138 - 1.38 g/L, the correlation coefficient was 0. 9995, the relative standard deviation （RSD） was 4. 2% （n = 8） and the detection limits （LOD） of n-hexane was 89. 2μg/L （but the LOD was 5.2 μg/L after LPME）. In addition, when the initial concentration of n-hexane was in the range of 0. 00346 - 0. 138 g/L, the enrichment factor of n-hexane decreased in a logarithmic type with the increase of its initial concentration, and this provided new evidence for theoretical research on LPME. When the method developed was applied to the analysis of adhesive samples, the average recoveries reached 92. 3% -96. 2% and the RSD was within the range of 3.6% -4. 7% （n =6）, which can fully meet the requirements for analysis of n-hexane in adhesive samples.

关 键 词：中空纤维 顶空液相微萃取 气相色谱 胶黏剂 正己烷 

分 类 号：O657.7[理学—分析化学]