超高效液相色谱-串联质谱法测定印刷电路板中全氟辛烷磺酸盐  

UHPLC-MS/MS Determination of Perfluoro-octane Sulfonate in Printed Circuit Boards

作　　者：曾泳艇[1] 幸苑娜[1] 陈泽勇[1] 李碧芳[1] 

机构地区：[1]深圳市计量质量检测研究院,深圳518109

出　　处：《理化检验（化学分册）》2011年第10期1159-1161,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：科技部创新方法工作资助项目(2008IM021800)

摘　　要：经剪碎和粉碎的印刷电路板样品用甲酸-甲醇(0.1+99.9)溶液超声提取,所得提取液于45℃旋转蒸发至1mL,加水5mL,用稀甲酸或稀氨水调节溶液的pH值为4～5。将溶液通过Oasis WAX固相萃取小柱净化,用甲酸(2+98)溶液和甲醇先后清洗小柱后,用氨水-甲醇(2+98)混合溶液洗脱,将全部洗脱液氮吹蒸发至近干,用流动相溶液定容为1mL供测定。所用色谱柱为Acquity UPLC BEH C18柱,柱温30℃,进样量为5μL。由5mmol.L-1乙酸铵溶液及乙腈(60+40)混合溶液作为流动相,在0.3mL.min-1流量条件下进行洗脱。质谱测定中采用ESI负电离方式,多反应监测扫描模式。测得全氟辛烷磺酸盐质量分数在1.0～1 000μg.kg-1范围内与峰面积值呈线性关系,测定下限(10S/N)为1.0μg.kg-1。用标准加入法测得回收率在89.0%～99.3%之间。An appropriate amount of cut and crushed printed circuit board （PCB） sample was taken and extracted with HCOOH-CH3OH（0. 1＋99.9） mixture ultrasonically. The extract was evaporated to ca. 1 mL in a rotary evaporator at 45 ℃, 5 mL of H20 was added and the pH value of the solution was adjusted to 4-5 with dil. formic acid and dil. aq. ammonia. The solution was then purified by passing through the Oasis WAX SPE micro column and eluting with mixture of NH3 （aq.）＋CH3 OH（2 ＋ 98）. The eluate was blown with N2 to near-dryness, and made up its volume to 1 mL with the mobile phase solution mentioned below. An aliquot of 5 μL of the sample was introduced for analysis. The Acquity UPLC BEH C18 column with column temp. of 30 ℃ was used for chromatographic separation, using a mixture of 5 mmol· L^-1 NH4OAc solution and acetonitrile（60＋40） as mobile phase for elution （flow-rate： 0.3 mL · min^-1 ）. ESI with negative ionization mode and scanning mode of MRM were used in the MS/MS analysis. Linearity range for perfluoro-octane sulfonate was found between 1.0～1000μg·kg^-1. Lower limit of determination （lOS/N） was found to be 1.0μg·kg^-1. Values of recovery found by standard addition method were in the range of 89.0%～99.3%.

关 键 词：超高效液相色谱-串联质谱 印刷电路板 全氟辛烷磺酸盐 

分 类 号：O652.63[理学—分析化学]