高效液相色谱-串联质谱法测定水中全氟辛烷磺酸含量

建立了水中全氟辛烷磺酸(perfluoro-rooctane sulfonate, PFOS)的高效液相色谱-串联质谱法分析方法。用0.22μm PP滤膜过滤水样,Poly-Sery HLB固相萃取柱对200 mL水样进行富集处理,以质量分数为10%的甲醇水溶液淋洗HLB柱以去除表面杂质,随后抽真空,再用4 mL纯甲醇溶液洗脱HLB柱。取洗脱液上机检测,以质量分数为0.1%的甲酸为流动相A,甲醇为流动相B,采用ACQΜITYΜPLC BEH C;色谱柱对洗脱液进行分离,负离子多反应监测模式检测,碎片离子m/z=80,内标法定量分析。在优化条件下,PFOS在0.01~50μg/L范围内线性较好,相关系数r>0.99,方法检出限为0.25μg/L。方法加标回收实验添加浓度0.2、2.0和20μg/L,PFOS加标回收率为82.1%~104.5%,相对标准偏差(RSD)为2.34%~5.64%。采集湖泊及养殖虾塘进出口水样进行测定,其PFOS含量均低于检出限,其中,湖水加标回收率为84.75%~112.2%,RSD<5.62%,养殖塘水样加标回收率为81.7%~118.6%,RSD<7.51%,实验所建方法可方便准确地检测水中PFOS含量。

Determination of perfluorooctane sulfonic acid in water by high performance liquid chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS)method or perfluorooctane sulfonic acid(PFOS) analysis in water was established. The water sample was pretreated with a 0.22 μm PP filter membrane, and then 200 mL pretreated water was enriched with a Poly-Sery HLB solid phase extraction column. The enriched extraction column was eluted by passing it through 10% aqueous methanol, after which the elution chamber was evacuated and the column was washed again with 4 mL methanol. And then ACQ MITY MPLC BEH C;chromatographic column was used to separate the eluent in the negative ion multi-reaction monitoring mode detection, fragment ion m/z=80, by internal standard method quantitative analysis, using a 0.1% formic acid aqueous solution-methanol solution as mobile phase. Under preferred conditions, PFOS was linear in the concentration range 0.01-50 μg/L with a correlation coefficient r>0.99, and the method limit of detection was 0.25 μg/L. The spiked recoveries ranged from 82.1% to 104.5% and the relative standard deviations(RSD) ranged from 2.34% to 5.64% for PFOS at the spiked concentrations of 0.2, 2.0, and 20 μg/L, respectively. The PFOS content in the actual water samples was below the detection limit, the lake water spiked recovery rate was between 84.75%-112.2%, RSD<5.62%, and the aquaculture water sample spiked recovery rate was between 81.7%-118.6%, RSD<7.51%. The established method can accurately detect PFOS in environmental water.