建立了一种高效液相色谱-串联质谱(HPLC-MS/MS)测定泡沫灭火材料、洗涤剂以及织物整理剂中全氟辛烷磺酸及其盐(PFOS)的方法.对应产品中的PFOS用水超声提取后,经固相萃取柱淋洗萃取,萃取液以乙腈-10 mmol/L 乙酸铵溶液(80∶20,v/v)为流动相进行HPLC分离,在负离子模式和多级反应监测(MRM)方式下进行测定.用两个子离子的相对丰度定性,外标法定量.PFOS的测定在0.002～0.1 mg/L 范围内线性关系良好(r~2=0.998);泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的加标回收率分别为93.4% ～103% ,93.2% ～102%和91.8% ～102% ,精密度(以相对标准偏差(RSD)计)分别为0.48% ～3.52% ,0.78% ～1.79%和0.47% ～3.47% ;方法的检出限均为2 mg/kg(0.000 2% )(信噪比(S/N)≥10),满足欧盟法规对泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的限量检测要求.该方法准确度和灵敏度高,前处理简单,可用于泡沫灭火材料、洗涤剂以及织物整理剂中PFOS的检测.
A novel method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for the determination of perfluorooctane sulfonates (PFOS) in the fire-fighting foam,detergents and fabric finishing agents.The PFOS residue was extracted with water at first by ultrasonic,then separated by high-speed centrifugation.The supernatant was purified by pre-conditioned solid phase extraction (SPE) micro-column,and the extract was filtrated through a membrane with 0.2 μm diameter.The filtrated liquid was analyzed by HPLC using acetonitrile-10 mmol/L ammonium acetate solution (80∶20,v/v) as mobile phase.The PFOS was detected by using negative electrospray ionization (ESI) on a tandem mass spectrometer in multiple reaction monitoring (MRM) mode.The qualitative analysis of the PFOS can be performed by using the relative abundance of two daughter ions of PFOS,and the quantitative analysis was performed by external standard method.The linear calibration curve was obtained in the range of 0.002-0.1 mg/L with a linear correlation coefficient (r~2) of 0.998.The spiked recoveries for PFOS in the fire-fighting foam,detergents and fabric finishing agents were 93.4% -103% ,93.2% -102% and 91.8% -102% with the relative standard deviation of 0.48% -3.52% ,0.78% -1.79% and 0.47% -3.47% ,respectively.And the detection limit for PFOS was 2 mg/kg (S/N≥10),which can meet the requirement for the PFOS restriction in fire-fighting foam,detergents and fabric finishing agents in the EU directives.With high accuracy and sensitivity,the method is simple and rapid,and can be used for PFOS inspection in fire-fighting foam,detergents and fabric finishing agents.
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