固相萃取-液相色谱/荧光检测法同时测定水中8种烷基酚和烷基酚聚氧乙烯醚

Simultaneous determination of eight alkylphenols and alkylphenol ethoxylates in water by solid phase extraction and high performance liquid chromatography with fluorescence detection

本文通过优化色谱条件、前处理条件、样品保存条件等,建立了水中8种烷基酚(APs)和烷基酚聚氧乙烯醚(APEOs)的固相萃取(SPE)—高效液相色谱/荧光检测(HPLC-FLD)分析方法.水样经酸化(p H 2.0—3.0)后加入甲醇至20%体积分数,并以10 m L·min^(-1)速度通过HLB固相萃取小柱进行浓缩和净化,收集SPE洗脱液进行HPLC-FLD检测分析.采用Waters PAH C18色谱柱(4.6×250 mm,5.0μm),以乙腈和5 mmol·L-1醋酸铵溶液进行梯度洗脱,流速为1.0 m L·min^(-1),荧光检测的激发和发射波长分别为228 nm和300 nm.结果表明,8种组分的线性关系良好(R>0.998),方法检出限为0.2—0.5μg·L-1.在低、中、高加标水平下,8种组分的回收率分别为82.5%—119.4%、92.1%—118.0%、89.7%—103.9%,平均相对标准偏差分别为5.3%、5.4%、2.9%.该方法灵敏度高、操作简单、易于推广应用,适用于水中多种APs与APEOs的同时分析.

This study presents a method for the simultaneous determination of eight alkylphenols（ APs） and alkylphenol ethoxylates（ APEOs） in water samples by solid phase extraction（ SPE） and high performance liquid chromatography with fluorescence detector（ HPLC-FLD）. Samples were acidified（ p H 2. 0—3. 0） and adjusted to containing 20% methanol before concentration and purification by HLB SPE cartridges. APs and APEOs were analyzed by liquid chromatography with PAH C18 chromatographic column（ 4. 6 × 250 mm,5. 0 μm） and fluorescence detector. The excitation wavelength and emission wavelength were 228 nm and 300 nm,respectively. Acetonitrile-5 mmol·L-1 ammonium acetate were used as the mobile phase with gradient elution at a flow rate of1 m L·min^（-1）. Results indicated that the method has a good linear relationship（ R0.998）. The limits of detection（ LODs） for eight APs and APEOs were 0. 2—0. 5 μg·L-1. The recoveries of eightanalytes at low,medium,and high spiked levels were 82. 5%—119. 4%,92. 1%—118. 0% and89.7%—103.9%,respectively. The corresponding average relative standard deviations（ RSD） were5.3%,5.4% and 2.9%,respectively. The method is simple,senvitive and easy to implement. It is suitable for the simultaneous detection of various APs and APEOs in water.