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
周昊昱 1龚孝铰 1蒋晶 1宋冰冰 2皇甫晓东 1王凌峰 1王国庆 3胡夏可 3唐瑶3
作者信息
- 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
- 折叠
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0～100 μg/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.
Abstract
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 parame-ters 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 devia-tion of the actual labeled samples of low,medium and high mass concentrations ranged from 0.53%to 12.00%,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Key words
PFCs detecting/water quality/solid phase extraction/HPLC-ESI-MS/MS引用本文复制引用
基金项目
2023年湖南省环保科研项目(HNKYXM-2023041)
出版年
2024
国家科技期刊平台
NSTL
万方数据