作　　者： ; ; ; ; ;

机构地区： 中国广州分析测试中心广东省化学危害应急检测技术重点实验室

出　　处： 《分析化学》 2007年第11期1591-1595,共5页

摘　　要： 建立了纺织品和皮革制品中全氟辛烷磺酸盐（PFOS）的液相色谱-二级质谱（LC-MS^2）测定方法。样品经0．1mol／L HCl和甲醇超声波振荡提取，高效液相色谱分离；色谱柱为ZorbaxSB-C18；流动相为V（甲醇）：V（10mmol／L乙酸铵水溶液）=70：30，流速为0．3mL／min。采用负离子模式的电喷雾质谱检测。以一级质谱得到的准分子离子m／z 499作为母离子，进行二级质谱（MS^2）分析。选择MS^2的碎片离子m／z 169、230、280、330及419定性确证，MS。总离子流色谱（TIC）峰面积定量。实验优化了样品提取方法和色谱、质谱条件，并对二级质谱碎裂机理和特征离子进行了研究。结果表明，本法简便快速，准确可靠，相对标准偏差小于8．6％，回收率在90％～99％之间；检出限为1．5mg／kg，远低于欧盟指令50mg／kg的限量规定。本方法已成功应用于纺织品、皮革制品中痕量PFOS的测定。 A method was established for the determination of perfluorooctane sulphonate（PFOS） in fabric and leather by liquid chromatography-mass spectrometry （LC-MS/MS）. PFOS in fabric and leather was extracted by 0.1 mol/L HCl andmethanol with ultrasonic wave. The extract was separated on a Zorbax SB-Cx8 column （2.1 mm × 150 mm, 3.5 μm） with methanol -10 mmol/L ammonium acetate（70：30） as the mobile phase at the flow rate of 0.3 mL/min, and determined by （ - ） ESI MS/MS. The conditions of extraction and LC- MS/MS were optimized. The parent ion of （ - ） ESI MS was m/z 499, and it＇s daughter ions of MS/MS m/z 169,230,280,330 and 419 were selected as qualitative. The TIC of MS/MS was selected as quantitative of PFOS. The PFOS recovery was in the range of 90% - 99% and the RSD was less than 8.6% , the limit of determination was 1.5 mg/kg. The method is simple and accurate, and has been applied to the determination of PFOS in fabric and leather.

关 键 词： 全氟辛烷磺酸盐 液相色谱 质谱 纺织品 皮革制品

领　　域： [理学] [理学]