新型毛细管内固相萃取-气相色谱法检测纺织品中烷基酚类物质  

Determination of alkyl-phenols in textiles by in-tube capillary solid-phase extraction-gas chromatography

作　　者：张洛红[1] 杜婷[1] 钟佳宇 

机构地区：[1]西安工程大学环境与化学工程学院,陕西西安710048

出　　处：《色谱》2015年第10期1065-1070,共6页Chinese Journal of Chromatography

基　　金：教育部留学回国人员科研启动基金([2010]1561);省教育厅科研专项(14JK1297);陕西省科技厅项目(2015XT-24)

摘　　要：建立了毛细管内固相萃取（SPE）-气相色谱（GC）检测纺织品中壬基酚和辛基酚含量的分析方法。通过比较4种性质不同固相萃取剂的萃取效果,筛选出对烷基酚（APs）类物质萃取效果最佳的固相萃取剂,将其作为填充物质制作毛细管内固相萃取柱,将毛细管内固相萃取法与气相色谱联用进行分析检测。最佳固相萃取剂为Abselut NEXUS,毛细管内固相萃取最佳条件为：1.2μL甲醇和1.2μL超纯水活化,1.2μL甲醇洗脱,上样速率是0.4μL/min。该法在较低浓度范围内呈现良好的线性相关性,对烷基酚的富集倍数约为100倍,对辛基酚和壬基酚的检出限分别为3.7μg/L和4.5μg/L,加标回收率分别为85.6%~98.2%和83.8%~95.7%,结果表明,此法能够简捷、迅速、有效地检测出纺织品中残留的烷基酚类物质。An in-tube capillary solid-phase extraction（SPE）-gas chromatography（GC）method was developed for confirmation and quantitative determination of octylphenol（OP） and nonylphenol（NP）in textiles. To make the in-tube capillary SPE column,the best SPE cartridge was chosen from four kinds of SPE cartridges. The adsorbent in the cartridge was used as the filling material to make the in-tube capillary SPE column. The nature,volume used,flow rate and adsorption capacity of the eluent were compared. Finally,the in-tube capillary solidphase extraction was combined with gas chromatography to detect the alkyl phenols（APs）.Abselut NEXUS extraction cartridge was chosen as the best solid phase extractant. The optimal in-tube capillary SPE extraction conditions were as follows：1. 2 μL methanol and 1. 2 μL ultrapure water for activating the extraction column,1. 2 μL methanol for eluting,0. 4 μL / min for solution loading. The method showed a good linear relationship in the low concentration range,and the enrichment ratios for the APs were about 100 times. The detection limits of octylphenol and nonylphenol were 3. 7 μg / L and 4. 5 μg / L,respectively. The recoveries of octylphenol were85. 6%-98. 2%,and those of nonylphenol were 83. 8%-95. 7%. The experimental results demonstrated that the method is simple,rapid,and useful for detecting APs in textiles.

关 键 词：毛细管内固相萃取法 气相色谱 烷基酚 辛基酚 壬基酚 纺织品 

分 类 号：O658[理学—分析化学]