固相萃取液相色谱-三重四极杆质谱仪测定水中7种烷基酚类和双酚类化合物  

Determination of Seven Alkylphenols and Bisphenol Compounds in Water by Solid Phase Extraction Liquid Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：甘杰 丰小阳 王国庆 蒋开年 熊芬 魏凤 GAN Jie;FENG Xiaoyang;WANG Guoqing;JIANG Kainian;XIONG Fen;WEI Feng(Hunan Ecological and Environmental Monitoring Center;Guojian Testing Holdings Group Hunan Huake Technology Co.,Ltd.,Changsha 410014,China;Hunan Yongzhou Ecological and Environmental Monitoring Center,Yongzhou 425000,China)

机构地区：[1]湖南省生态环境监测中心 [2]国检测试控股集团湖南华科科技有限公司,长沙410014 [3]湖南省永州生态监测中心,湖南永州425000

出　　处：《中国资源综合利用》2025年第2期16-23,共8页China Resources Comprehensive Utilization

基　　金：湖南省环保科研课题(HBKT-2002006);国家可持续发展议程创新示范区建设省级专项(2021sfq26)。

摘　　要：试验通过优化前处理过程和质谱条件等方式,提出一种利用高效液相色谱法分析水中7种烷基酚类(辛基酚、4-辛基酚、壬基酚、4-壬基酚)和双酚类化合物(双酚A、双酚B、双酚F)的方法。采用孔径0.45 μm的石英滤膜过滤样品,利用苯乙烯/二乙烯苯共聚物色谱柱固相萃取小柱对样品进行前处理。柱温设定为40 ℃,流速设定为0.3 mL/min,以甲醇和氨水为流动相,利用梯度洗脱进行分离,采用液相色谱-串联质谱多反应监测(Multiple Reaction Monitoring,MRM)负离子模式测定,运用内标法定量。结果显示,在0.1~50.0 μg/L浓度检测范围内,7种烷基酚类和双酚类化合物标准曲线线性良好(相关系数r>0.999)。低、中、高3种浓度加标样品的相对标准偏差保持在2.6%~17.2%,回收率为75%~102%,方法检出限为0.000 06~0.000 10 μg/L。测试结果表明,该方法可适用于地表水、地下水以及饮用水的实际检测工作。In this experiment,a method for analyzing seven alkylphenols (octylphenol,4-octylphenol,nonylphenol,4-nonylphenol) and bisphenol compounds (bisphenol A,bisphenol B,bisphenol F) in water using high-performance liquid chromatography is proposed by optimizing the pretreatment process and mass spectrometry conditions.The sample is filtered using a quartz filter membrane with a pore size of 0.45 μm,and the sample is pretreated using a styrene/divinylbenzene copolymer chromatography column solid-phase extraction column.The column temperature is set to 40 ℃,the flow rate is set to 0.3 mL/min,methanol and ammonia water are used as mobile phases,and gradient elution is used for separation,and liquid chromatography tandem mass spectrometry Multiple Reaction Monitoring (MRM) negative ion mode is used for determination,and internal standard method is used for quantification.The results show that within the concentration detection range of 0.1~50.0 μg/L,the standard curves of 7 alkylphenols and bisphenol compounds show good linearity (correlation coefficient r>0.999).The relative standard deviation of the spiked samples with low,medium,and high concentrations remained between 2.6% and 17.2%,the recovery rate ranged from 75% to 102%,and the method detection limit was 0.000 06~0.000 10 μg/L.The test results indicate that this method is suitable for practical detection of surface water,groundwater,and drinking water.

关 键 词：固相萃取 高效液相色谱 三重四极杆质谱仪 烷基酚 双酚 

分 类 号：X834[环境科学与工程—环境工程] O657.7[理学—分析化学]