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固相萃取净化-正相高效液相色谱测定纺织品中残留的烷基酚和烷基酚聚氧乙烯醚

Determination of alkylphenols and alkylphenol polyethoxylates in textiles by normal-phase high performance liquid chromatography and solid-phase extraction

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【作者】 吕春华陈笑梅刘海山

【Author】 Lü Chunhua,CHEN Xiaomei,LIU Haishan(Zhejiang Entry-Exit Inspection and Quarantine Bureau,Hangzhou 310012,China)

【机构】 浙江出入境检验检疫局

【摘要】 建立了测定纺织品中烷基酚(AP)和烷基酚聚氧乙烯醚(APnEO)(n=2~16)的正相高效液相色谱法。以甲醇为提取溶剂,用索氏抽提法提取纺织品中的AP和APnEO,用正相高效液相色谱法测定,并对提取溶剂、提取方式和净化条件等前处理条件进行优化。该方法的检出限为1.0mg/kg,回收率为90.4%~104.1%,相对标准偏差为0.64%~4.21%。采用该方法对多种基质纺织品进行检测,可满足残留检测要求。

【Abstract】 A method for the simultaneous determination of alkylphenols(AP)and alkylphenol polyethoxylates(APnEO)(n=2-16)in textiles was developed by normal-phase high performance liquid chromatography(NP-HPLC).The residues of AP and APnEO in the samples were extracted with methanol by Soxhlet extraction.The pretreatment conditions such as extraction solvents,extraction methods and clean-up methods were optimized.The sample was purified by an HLB solid-phase extraction column and separated on an amino column(250 mm×4.6 mm,5 μm)with hexane-isopropanol(90∶10,v/v)and isopropanol-water(90∶10,v/v)as mobile phases at a flow rate of 1.0 mL/min and determined by a fluorescence detector.AP and each APnEO oligomer were separated successfully within a reasonable time with gradient elution,which are difficult to be separated by using conventional reversed-phase high performance liquid chromatography(RP-HPLC).The detection limit was 1.0 mg/kg for each analyte.The recoveries ranged from 90.4% to 104.1% with the relative standard deviations(RSDs)ranged from 0.64% to 4.21%.This method is suitable for the determination of alkylphenols and alkylphenol polyethoxylates in textiles.

【基金】 浙江省国境安全检验检疫科技创新服务平台(项目编号:2006C17014)
  • 【文献出处】 色谱 ,Chinese Journal of Chromatography , 编辑部邮箱 ,2009年04期
  • 【分类号】TS107
  • 【被引频次】22
  • 【下载频次】341
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