地毯中全氟辛烷磺酰基化合物_PFOS_的测定方法研究.pdfVIP

检验·论坛 Inspection. Forum 地毯中全氟辛烷磺酰基化合物 （PFOS）的 测定方法研究 Determination of Perfluorooctane Sulfonates(PFOS) in Carpet 文/ 卢晓东 于丽华 郝永 高会兰 摘要 本文利用高效液相色谱－电喷雾串联质谱(HPLC －E SI-M S/M S)技术研究地毯中全氟辛烷磺酰基化合物 (PFOS)的测定方法。地毯样品采用超声波辅助萃取，萃取液经0.2µm有机滤膜过滤后，以42：58(体积比)的甲醇 5mmol/L 乙酸铵溶液为流动相，经HPLC分离后用多级反应监测(MRM)模式测定。用两个子离子的相对丰度定 性，外标法定量。结果表明，PFOS在0.002~0.1 mg/L 范围内线性良好(r ＞0.999 5) ，回收率大于90 ％，相对标准 偏差小于2 ％。满足欧盟法规对产品中PFOS的限量检测要求。 关键词：高效液相色谱 电喷雾串联质谱(HPLC—ESI-MS/MS) ；全氟辛烷磺酰基化合物 （PFOS）；地毯 － Abstract ：A novel method based on high performance liquid chromatography—tandem mass spectrometry(HPLC-ESI- MS/MS)combined with electron spray ionization was developed for quantitative detection of trace perfluorooctane sulfonate (PFOS) in carpet. Carpet samples were extracted by ultrasonic and the extract was fihrated through membrane with diameter of 0.2µm. The filtration liquid was determined by HPLC using 42:58 (by volume) methanol-5mmol/L ammonium acetatesolution as mobile phase. The PFOS was detected under multiple reactions monitoring (MRM) mode. Qualitative analysis of the PFOS could be performed using the relative abundance of two daughter ions of PFOS, and quantitative analysis was conducted with external standard method. The linear calibration curve was obtained in the range of 0.002~0.1mg/L with a correlation coefficient more than 0.9995. The spiked recoveries of PFOS was higher than 90 ％with RSD less than 2%. The method could be used for PFO