固相萃取-高效液相色谱-荧光检测法快速测定水中9种烷基酚和双酚A  

Rapid Determination of 9 Alkylphenols and Bisphenol A in Water by Using Solid-Phase Extraction-High Performance Liquid Chromatography-Fluorescence Detection

作　　者：王斐 郭晋君 张新颖 周弛 张会强 张秦铭 田渭花 WANG Fei;GUO Jin-jun;ZHANG Xin-ying;ZHOU Chi;ZHAN Hui-qiang;ZHANG Qin-ming;TIAN Wei-hua(Shaanxi Key Laboratory of Environmental Monitoring and Forewarning of Trace Pollutants,Shaanxi Environmental Monitoring Center,Xi′an 710054,China;College of Urban and Environmental Sciences,Northwest University,Xi′an,710127,China)

机构地区：[1]陕西省环境监测中心站陕西省环境介质痕量污染物监测预警重点实验室,陕西西安710054 [2]西北大学城市与环境学院,陕西西安710127

出　　处：《化学试剂》2024年第10期72-77,共6页Chemical Reagents

基　　金：陕西省重点研发计划项目(2023-YBSF-296);陕西省环境介质痕量污染物监测预警重点实验室开放课题项目(SHJKFJJ202307)。

摘　　要：建立了一种基于固相萃取-高效液相色谱-荧光检测技术快速测定实际水样中9种痕量烷基酚类化合物和双酚A的方法。首先筛选出能高分离度分离10种目标物的色谱柱,并进一步优化了柱温、检测波长、流动相流速和梯度时间等色谱条件。实现了10.0 min内快速分离检测10种目标物,显著提高了色谱分析流程的分离效果和检测效率。10种目标物在0.08(0.16)~10.00μg/L浓度范围内工作曲线线性关系良好,相关系数均大于0.998。方法检出限为0.02~0.04μg/L,定量限为0.08~0.16μg/L。地下水、地表水和工业废水的加标回收率分别为81.4%~98.0%、88.9%~103.0%和77.3%~107.8%,相对标准偏差为1.5%~7.3%、1.8%~5.6%和3.0%~7.4%。方法分析速度快、灵敏度好、重现性好、准确度高,能够用于实际水样中烷基酚类化合物和双酚A的测定。A method for the rapid determination of nine trace alkylphenols and bisphenol A in real water samples was established using solid-phase extraction combined with high-performance liquid chromatography and fluorescence detection.A chromatographic column capable of highly resolving 10 target substances was selected.Chromatographic conditions such as column temperature,detection wavelength,mobile phase flow rate,and gradient time were further optimized.The 10 target substances were rapidly separated and detected within 10.0 minutes,which significantly improved the separation effect and detection efficiency of the chromatographic analysis process.The calibration curves showed good linearity(r>0.998)for the 10 target analytes in the range of 0.08(0.16)~10.00μg/L.The method detection limits ranged from 0.02 to 0.04μg/L,and the quantification limits ranged from 0.08 to 0.16μg/L.The recoveries in spiked groundwater,surface water,and industrial wastewater,were in the range of 81.4%~98.0%,88.9%~103.0%,and 77.3%~107.8%,respectively,with the relative standard deviations of 1.5%~7.3%,1.8%~5.6%,and 3.0%~7.4%.This method features fast analysis speed,high sensitivity,reproducibility,and accuracy,making it suitable for the determination of alkylphenols and bisphenol A in real water samples.

关 键 词：烷基酚 双酚A 快速测定 实际水样 高效液相色谱 

分 类 号：O657.7[理学—分析化学]