柱上衍生-气相色谱-质谱法测定纺织织物中的痕量全氟辛基磺酸

摘要

A novel method for the determination of trace perfluorooctane sulfonic acid (PFOS) in water and oil repellent fabrics was developed using on-column derivatization/gas chromatography/mass spectrometry (GC/MS) with ultrasonic-microwave synergistic extraction as the pretreatment method.While the tetrabutylammonium hydroxide (TBAH) was used as the derivative reagent via an in situ pyrolytic alkylation reaction with PFOS occurred on the GC column,the butyl PFOS derivative was generated and then separated effectively and analyzed by gas chromatography/mass spectrometry under SIM mode.The characteristic ions were as follows m/z 57,69,131,169,449.The average recovery was between 83.6％ and 91.7％,the relative standard deviation (RSD) was less than 7.3％ and the detection limit was 58.8 μg/L.The amounts of PFOS in the textile samples were detected in the range from 0.063 to 13.9 mg/kg by this method.%立了柱上衍生-气相色谱-质谱法测定憎水憎油纺织织物中痕量全氟辛基磺酸(PFOS)的检测方法,运用超声-微波协同提取技术,使用四丁基氢氧化铵(TBAH)为衍生化试剂,与PFOS形成铵盐,并在柱上进行原位裂解烷基化反应,所得PFOS丁酯利用气相色谱-质谱法进行分离和分析,采用选择离子(SIM)模式检测,特征离子分别为m/z 57,69,131,169和449.本方法的加标回收率为83.6％～91.7％,相对标准偏差(RSD)小于7.34％,检出限为59 mg/L.运用本法对憎水憎油纺织织物样品进行检测,PFOS含量在0.063～ 13.9 mg/kg之间.