首页|固相萃取-HPLC-ESI-MS/MS法测定水中全氟化合物

固相萃取-HPLC-ESI-MS/MS法测定水中全氟化合物

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

PFCs detectingwater qualitysolid phase extractionHPLC-ESI-MS/MS

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

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湖南省永州生态环境监测中心,湖南永州 425000

湖南省生态环境监测中心,湖南长沙 410116

国检测试控股集团湖南华科科技有限公司,湖南长沙 410021

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

2023年湖南省环保科研项目

HNKYXM-2023041

2024

印染助剂
江苏苏豪传媒有限公司

印染助剂

CSTPCD
影响因子:0.476
ISSN:1004-0439
年,卷(期):2024.41(7)
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