摘要
建立填充吸附微萃取-气相色谱-质谱法测定水中12种酚类化合物。将样品溶液pH值调节至2,选择HLB为萃取材料,以15μL/s流量萃取30次,用500μL水冲洗萃取柱,抽取500μL空气吹扫HLB萃取柱20次去除水分,用100μL含0.2%甲酸的乙腈溶液洗脱,在优化的仪器工作条件下测定洗脱液,用外标法定量。12种酚类化合物在30min内分离良好,其质量浓度在0.05~10 mg/L范围内与色谱峰面积线性关系良好,相关系数为0.993~0.999 7,方法检出限为0.2~2μg/L,定量限为0.8~8μg/L。空白样品加标平均回收率为77.9%~111%,测定结果的相对标准偏差为3.4%~14%(n=6)。该方法适用于水中酚类化合物的快速测定。
A method for the determination of 12 phenolic compounds in water was established using microextraction by packed sorbent coupled with gas chromatography-mass spectrometry.The pH value of the sample solution was adjusted to 2,HLB as the extraction material,30 extraction cycles at a flow rate of 15μL/s,the extraction column was rinsed with 500μL of pure water.The HLB extraction column was dried with 500μL of air for 20 times to remove moisture,and elution with 100μL of acetonitrile solution containing 0.2%formic acid.The eluent was determined under optimized instrument operating conditions and quantify using external standard method.The 12 phenolic compounds were well separated within 30 minutes,with their mass concentration had good linear relationship with the chromatographic peak area in the range of 0.05-10 mg/L,and the correlation coefficients of 0.993-0.9997.The detection limits of the method were 0.2-2μg/L,and the quantification limits were 0.8-8μg/L.The average recoveries of blank samples spiked were 77.9%-111%,and the relative standard deviations of the determination results for six parallel samples were 3.4%-14%.This method is suitable for rapid determination of phenolic compounds in water bodies.
作者
何莲
冯加永
屈晓萍
王巧玲
杨明光
张苗苗
陈芹
梁金鑫
唐剑锋
HE Lian;FENG Jiayong;QU Xiaoping;WANG Qiaoling;YANG Mingguang;ZHANG Miaomiao;CHEN Qin;LIANG Jinxin;TANG Jianfeng(Zhejiang Zhekan Testing Co.,Ltd.,Ningbo 315033,China;Zhejiang Ningbo Ecological and Environmental Monitoring Center,Ningbo 315048,China;Ningbo Urban Environment Observation and Research Station,Chinese Academy of Sciences,Ningbo 315800,China)
出处
《化学分析计量》
2026年第1期8-15,共8页
Chemical Analysis And Meterage
基金
国家自然科学基金项目(31971489)
2025年度第一批宁波市“科创甬江2035”重点研发计划项目(2025Z022)
浙江省工程勘察设计院集团有限公司科研项目(202102)。
关键词
填充吸附微萃取
气相色谱-质谱法
酚类化合物
水质
microextraction by packed sorbent
gas chromatography-mass spectrometry
phenolic compounds
water
