色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1065-1070.DOI: 10.3724/SP.J.1123.2015.05003

• 研究论文 • 上一篇    下一篇

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

张洛红, 杜婷, 钟佳宇   

  1. 西安工程大学环境与化学工程学院, 陕西 西安 710048
  • 收稿日期:2015-05-07 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 杜婷
  • 基金资助:

    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).

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

ZHANG Luohong, DU Ting, ZHONG Jiayu   

  1. College of Environmental and Chemical Engineering, Xi'an Polytechnic University, Xi'an 710048, China
  • Received:2015-05-07 Online:2015-10-08 Published:2012-05-09

PDF

100

被引次数

14

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:1.2 μL甲醇和1.2 μL超纯水活化,1.2 μL甲醇洗脱,上样速率是0.4 μL/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3.7 μg/L和4.5 μg/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。

关键词: 纺织品, 毛细管内固相萃取法, 气相色谱, 壬基酚, 烷基酚, 辛基酚

Abstract:

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 solid-phase 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 were 85.6%-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.

Key words: alkyl phenols (APs), gas chromatography (GC), in-tube capillary solid-phase extraction (SPE), nonylphenol, octylphenol, textile

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