Wang X F, Wang Q, Li Z G, Huang K, Li L D, Zhao D H
a Key Laboratory of Aquatic Product Processing, Ministry of Agriculture , Guangzhou , China.
b Lab. of Quality & Safety Risk Assessment for Aquatic Product on Storage and Preservation (Guang Zhou) , Guangzhou , China.
J Environ Sci Health A Tox Hazard Subst Environ Eng. 2018;53(14):1277-1283. doi: 10.1080/10934529.2018.1528042. Epub 2019 Jan 9.
A practical multi-residue method based on ultra-performance liquid chromatography/tandem mass spectrometry was developed for the simultaneous determination of 23 perfluorinated alkylated substances (PFASs) in water and suspended particles. Suspended particle samples were extracted with 1% formic acid-acetonitrile and cleaned by matrix solid phase dispersion extraction using a C sorbent and graphitized carbon black. Water samples were filtered through 0.7-μm glass fiber membranes and enriched utilizing weak anion exchange cartridges. The eluent was dried under a gentle stream of N at 45°C and suspended in 1 mL acetonitrile-5 mM ammonium acetate (1:1, vol:vol). Gradient elution for chromatographic separation utilized acetonitrile and 5 mM ammonium acetate as mobile phases on a reverse phase C column. The compounds were quantified using an internal standard method in multiple reaction-monitoring mode. Limits of detection and quantitation of the 23 PFAS test compounds in water samples were 0.5-10 ng L and 2-20 ng L, respectively. Recoveries at three fortified levels of 20, 50, and 200 ng L ranged from 68.5% to 118% with relative standard deviations below 9.6%. We used this method to determine PFAS levels in real water and suspended particle samples and found high sensitivity and good reproducibility.
建立了一种基于超高效液相色谱/串联质谱的实用多残留方法,用于同时测定水和悬浮颗粒中的23种全氟烷基化物质(PFASs)。悬浮颗粒样品用1%甲酸-乙腈萃取,并用C吸附剂和石墨化炭黑通过基质固相分散萃取进行净化。水样通过0.7μm玻璃纤维膜过滤,并用弱阴离子交换柱进行富集。洗脱液在45℃下用N2缓流吹干,然后悬浮于1mL乙腈-5mM醋酸铵(1:1,体积比)中。色谱分离采用梯度洗脱,以乙腈和5mM醋酸铵为流动相,在反相C柱上进行。化合物在多反应监测模式下采用内标法进行定量。水样中23种PFAS测试化合物的检测限和定量限分别为0.5-10ng/L和2-20ng/L。在20、50和200ng/L三个加标水平下的回收率为68.5%-118%,相对标准偏差低于9.6%。我们用该方法测定了实际水样和悬浮颗粒样品中的PFAS水平,发现其具有高灵敏度和良好的重现性。