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用正相高效液相色谱法和固相萃取法测定纺织品中的烷基酚和烷基酚聚乙氧基化物

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

作者信息

Lü Chunhua, Chen Xiaomei, Liu Haishan

机构信息

Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou, China.

出版信息

Se Pu. 2009 Jul;27(4):458-62.

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 x 4.6 mm, 5 microm) 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.

摘要

建立了一种采用正相高效液相色谱法(NP-HPLC)同时测定纺织品中烷基酚(AP)和烷基酚聚氧乙烯醚(APnEO,n = 2 - 16)的方法。通过索氏提取法用甲醇提取样品中的AP和APnEO残留。对提取溶剂、提取方法和净化方法等预处理条件进行了优化。样品经HLB固相萃取柱净化后,在氨基柱(250 mm×4.6 mm,5 μm)上以正己烷 - 异丙醇(90:10,v/v)和异丙醇 - 水(90:10,v/v)为流动相,流速为1.0 mL/min进行分离,并用荧光检测器测定。通过梯度洗脱,AP和各APnEO低聚物在合理时间内成功分离,而使用传统反相高效液相色谱法(RP-HPLC)则难以分离。各分析物的检测限为1.0 mg/kg。回收率在90.4%至104.1%之间,相对标准偏差(RSD)在0.64%至4.21%之间。该方法适用于测定纺织品中的烷基酚和烷基酚聚氧乙烯醚。

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