Lü Chunhua, Chen Xiaomei, Liu Haishan
Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou, China.
Se Pu. 2009 Jul;27(4):458-62.
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.
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。
