离子液体分散液液微萃取-超高效液相色谱-串联质谱法测定食品接触材料中全氟辛酸和全氟辛烷磺酸的迁移量

Determination of migration of perfluorooctanoic acid and perfluorooctane sulfonic acid from food contact materials by ionic liquid-based dispersive liquid-liquid microextraction and ultra-performance liquid chromatography-tandem mass spectrometry

建立了一种基于离子液体分散液液微萃取前处理技术的食品接触材料中全氟辛酸和全氟辛烷磺酸迁移量的超高效液相色谱-串联质谱测定方法。水、10%(体积分数)乙醇溶液和4%(体积分数)乙酸溶液作为3种水性食品模拟物与食品接触材料充分接触,进行迁移试验,对迁移液采用离子液体分散液液微萃取技术进行目标物的萃取富集,考察了萃取剂种类和用量、涡旋时间、盐浓度、离心速率及时间等关键因素对食品模拟物中全氟辛酸和全氟辛烷磺酸萃取效率的影响。使用Waters ACQUITY UPLC BEH Shield RP18色谱柱(50 mm×2.1 mm,1.7μm),以乙腈和水为流动相,梯度洗脱分离,在电喷雾负离子模式下,采用多反应监测模式进行定性及定量分析。结果表明,全氟辛酸和全氟辛烷磺酸在各自范围内线性关系良好(r^2>0.99),检出限分别为0.5和1μg/L,定量限分别为2和5μg/L;在低、中、高3个添加水平下全氟辛酸和全氟辛烷磺酸的平均回收率为86.4%~116.9%,相对标准偏差为4.3%~14.4%(n=6)。该方法准确高效、环境友好,适用于食品接触材料中全氟辛酸和全氟辛烷磺酸迁移量的检测。

A new method was developed to determine the migration of perfluorooctanoic acid(PFOA)and perfluorooctane sulfonic acid(PFOS)from food contact materials(FCMs)using ionic liquid-based dispersive liquid-liquid microextraction(IL-DLLME)coupled with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).FCM samples were soaked in three food simulants of water,10%(v/v)aqueous ethanol solution,and 4%(v/v)acetic acid solution for the migration test,and then the migration liquid was extracted and enriched using the IL-DLLME.The key parameters in terms of the type and volume of extractant,vortex time,NaCl concentration,and the speed and time of centrifugation were investigated.The analytes were separated on a Waters ACQUITY UPLC BEH Shield RP18 column(50 mm×2.1 mm,1.7μm),eluted by gradient with acetonitrile and water,and quantified by electrospray ionization mass spectrometry in negative mode using multiple reaction monitoring(MRM).The experimental results showed good linearities(r 2>0.99)in their concentration ranges.The limits of detection(LODs)were 0.5 and 1μg/L,and the limits of quantitation(LOQs)were 2 and 5μg/L for PFOA and PFOS,respectively.The recoveries of PFOA and PFOS ranged from 86.4%to 116.9%at three spiked levels with the relative standard deviations(RSDs)between 4.3%and 14.4%(n=6).The proposed method was demonstrated as accurate,efficient,eco-friendly,and suitable for the determination of the migration of PFOA and PFOS from FCMs.