固相萃取-HPLC-ESI-MS/MS法测定水中全氟化合物  

Determination of seventeen perfluorinated compounds in water by solid phase extraction coupled with HPLC-ESI-MS/MS

作　　者：周昊昱 龚孝铰 蒋晶 宋冰冰 皇甫晓东 王凌峰 王国庆 胡夏可 唐瑶 ZHOU Haoyu;GONG Xiaojiao;JIANG Jing;SONG Bingbing;HUANGFU Xiaodong;WANG Lingfeng;WANG Guoqing;HU Xiake;TANG Yao(Hunan Yongzhou Ecological Environmental Monitoring Center,Yongzhou 425000,China;Hunan Ecological Environmental Monitoring Center,Changsha 410116,China;Hunan Huake Technology Co.Ltd.of National Inspection and Testing Holdings Group,Changsha 410021,China)

机构地区：[1]湖南省永州生态环境监测中心,湖南永州425000 [2]湖南省生态环境监测中心,湖南长沙410116 [3]国检测试控股集团湖南华科科技有限公司,湖南长沙410021

出　　处：《印染助剂》2024年第7期62-70,共9页Textile Auxiliaries

基　　金：2023年湖南省环保科研项目(HNKYXM-2023041)。

摘　　要：搭建了固相萃取-超高效液相色谱-电喷雾-串联质谱仪,发现测定水中17种全氟化合物(PFCs)的检测方法。采用玻璃纤维滤膜过滤样品,WAX萃取柱(固相萃取小柱)对样品进行前处理后,柱温和流速分别设定为40℃和0.3 mL/min,使用乙酸铵和乙腈作为流动相,利用梯度洗脱程序进行分离,超高效液相色谱-串联质谱多反应监测(MRM)负离子模式测定,内标法定量。通过优化实验的样品前处理条件和测试参数,标准曲线绘制结果显示,在0~100μg/L范围内,17种全氟化合物线性良好(R大于0.999)。低、中、高3种质量浓度的实际加标样品的相对标准偏差在0.53%~12.00%,回收率在70.7%~114.0%。测试结果表明该方法可以应用于实际检测工作。A method for the determination of 17 kinds of perfluorinated compounds(PFCs) in water was established by solid phase extraction,ultra-high performance liquid chromatography-electrospray series mass spectrometer.The samples were filtered by glass fiber filter membrane and pre-treated with WAX extraction column solid phase extraction column.The column temperature and the flow rate were set at 40 ℃ and 0.3 mL/min.Ammonium acetate and acetonitrile were used as mobile phases for separation by gradient elution procedure,and the samples were determined by UHPLC-tandem mass spectrometry(MRM) negative ion mode.Quantitative by internal standard method.By optimizing the conditions of pretreatment and test parameters of the experiment,the standard curve drawing results showed that the linearity of the method was good(R>0.999) for 17 kinds of perfluorinated compounds in the range of 0-100 μg/L.The relative standard deviation of the actual labeled samples of low,medium and high mass concentrations ranged from 0.53% to12.00%,and the recovery rate ranged from 70.7% to 114.0%.The test results showed that the method could be applied to the actual detection work.

关 键 词：全氟化合物检测 水质 固相萃取法 超高效液相色谱-电喷雾-串联质谱联用 

分 类 号：O657[理学—分析化学]