SPE-LC-MS/MS测定快餐纸袋中7种全氟有机物

徐睿; 谭红; 杨鸿波; 孙海达; 何锦林

doi:10.13386/j.issn1002-0306.2015.06.001

SPE-LC-MS/MS测定快餐纸袋中7种全氟有机物

Determination of seven perfluorinated compounds in fast food papers by solid phase extraction couple with solid phase extraction and liquid chromatography-mass spectrometry

摘要

摘要: 建立了快餐纸袋中7种全氟有机物（全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟十二烷酸、全氟十四烷酸、全氟辛烷磺酸盐）残留的固相萃取-液相色谱串联质谱（SPE-LC-MS/MS）分析方法。样品以1%甲酸-甲醇溶液超声提取,经C18固相萃取小柱净化,以0.1%甲酸乙腈-2mmol/L乙酸铵水溶液为流动相,经C8反相色谱柱分离,采用多反应监测（MRM）负离子模式检测,外标法定量。阴性样品添加实验表明:方法的检出限为0.008⁰.104μg/kg（S/N=3）;平均回收率为:80.2%¹06.0%;相对偏差为:2.2%⁸.1%（n=6）。该方法前处理简单,回收率高,精密度高,适用于各类快餐纸袋中全氟化合物的定量检测,为食品接触材料中全氟有机物的定量检测提供了方法。

Abstract: A method was established for the determination of 7 perfluorinated compounds( PFCS), including perfluorohexanoicacid(PFHx A),perfluoroheptanoic acid(PFHp A),perfluorooctanoic acid(PFOA),perfluorononanoic acid( PFNA), perfluorododecanoic acid( PFDo A), perfluorotetradec- anoic acid( PFTA), perfluorooctane sulphonate(PFOS) in fast food papers by solid phase extraction coupled with solid phase extraction and liquid chromatography- mass spectrometry( SPE- LC- MS / MS). Samples were extracted with 1 % formic acid-methanol by ultrasonic wave and cleaned up on C18 SPE column. 7 PFCs were separated on a C8reversed-phase column using gradient elution with acetonitrile and 2mmol / L ammonium acetate and analyzed by LC-MS/MS ESI(-) under MRM mode with the external standard phase. The results showed that four kinds of PFCs were detected. The limits of detection,average recovery rates,and the RSD(n=6) were 0.008~0.104μg/kg,80.2%~106.0%,2.2%~8.1%,respectively. The method was simple,accurate and sensitive for the determination and confirmation of PFCs in fast food papers and other materials used as food packaging.