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建立了蛋挞锡纸中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-2 mmol/L的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。通过阴性样品添加试验表明:方法的检出限为0.03~0.06μg/kg;平均回收率为:82%~117%;相对偏差为:1.8%~5.1%(n=6)。该方法前处理简单,回收率高,精密度好,适用于蛋挞锡纸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。
Seven types of perfluorinated organic compounds (perfluorohexanoic acid, perfluoroheptanoic acid, perfluorooctanoic acid, perfluorononanoic acid, perfluorododecanoic acid, perfluorotetradecanoic acid and perfluorooctane sulfonate) were established in the tin tart paper. Residual solid phase extraction - liquid chromatography tandem mass spectrometry (SPE-LC-MS / MS) analysis. The sample was extracted with 1% formic acid in methanol and purified by C18 solid phase extraction cartridge. The sample was separated on a C8 reversed-phase column using 0.1% formic acid in acetonitrile-2 mmol / L ammonium acetate as mobile phase. Multiple reaction monitoring (MRM) Negative ion mode detection, external standard method. Addition of negative samples showed that the detection limit was 0.03 ~ 0.06μg / kg. The average recovery was 82% ~ 117%. The relative deviation was 1.8% ~ 5.1% (n = 6). The method has the advantages of simple pretreatment, high recovery rate and good precision, and is suitable for the quantitative detection of perfluorinated compounds in egg tart paper foil, and provides a method for the quantitative detection of perfluoroorganic compounds in food contact materials.