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建立了爆米花桶中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%甲酸甲醇超声提取,经C18固相萃取小柱净化,以0.1%甲酸乙腈-2mmol/L的乙酸铵水溶液为流动相,经C18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。通过阴性样品添加实验表明:方法的检出限为0.03~0.52μg/kg(S/N=3);平均回收率为:88%~110%;相对偏差为:1.7%~5.0%(n=6)。该方法前处理简单,回收率高,精密度好,适用于爆米花桶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测定提供了方法。
A total of seven perfluorinated organic compounds (perfluorohexanoic acid, perfluoroheptanoic acid, perfluorooctanoic acid, perfluorononanoic acid, perfluorododecanoic acid, perfluorotetradecanoic acid, perfluorooctane sulfonate ) Residual SPE-LC-MS / MS method. The samples were extracted with 1% formic acid in methanol and purified by C18 solid phase extraction cartridges. The mobile phases were eluted with 0.1% formic acid in 2 mmol / L ammonium acetate aqueous solution and separated by C18 reversed-phase column. Multiple reaction monitoring (MRM) Negative ion mode detection, external standard method. The results showed that the detection limit of the method was 0.03-0.52μg / kg (S / N = 3), the average recovery was 88% -110% and the relative deviation was 1.7% -5.0% (n = 6). The method has the advantages of simple pretreatment, high recovery and good precision, and is suitable for the quantitative detection of perfluoro compounds in popcorn bucket, and provides a method for the determination of perfluoroorganic compounds in food contact materials.