Determination of 17 Perfluorinated Compounds in Soil and Sediment with Liquid Lhromatography-Tandem High-Resolution Mass Spectrometry
A detection method was established for the simultaneous determination of 17 perfluorinated compounds in soil and sediment through the ultrasound extraction solid-phase extraction/liquid chromatography-tandem high-resolution mass spectrometry.After orthogonal experiments on the extraction efficiency of perfluorinated compounds by designing extraction solvents,ultrasound temperature,ultrasound time,and ultrasound frequency,the optimal pre-treatment conditions were determined as follows:the sample was sieved through an 80 mesh sieve,ultrasonically extracted with methanol at 30℃ for 30 minutes;the supernatant was separated and concentrated to 1～2 mL,diluted to 200 mL with pure water,purified by PWAX solid-phase extraction column,and eluted with 0.05％ammonia-methanol solution.After the eluent was concentrated and adjusted to a constant volume,gradient separation was performed on an AcclaimTM VANQUISH C18 column by using 2 mmol/L ammonium acetate solution and acetonitrile as mobile phases.High resolution mass spectrometry was used for full scan quantitative analysis.The results showed that 17 perfluorinated compounds had good linearity within the mass concentration range of 1.0 μg/L to 20.0 μg/L,the correlation coefficient r was within the range of 0.997 to 0.9999,the detection limit was 0.1 μg/kg to 0.3 μg/kg,the lower limit was 0.4 μg/kg to 1.2 μg/kg,the spike recovery of samples was 96.8％～127％,and the relative standard deviation was 0.8％～9.1％.This method is featured by high efficiency,sensitivity and accuracy,and can be used for simultaneously monitoring 17 perfluorinated compounds in soil and sediments.
Perfluorinated compoundssoil and sedimentsliquid chromatography-tandem high-resolution mass spectrometryultrasonic extraction-solid phase extraction
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维普
