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[基于离子液体的分散液液微萃取和超高效液相色谱-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].

作者信息

Yan Mengmeng, Chen Meng, Meng Xianshuang, Guo Xiangyu, Bai Hua, Ma Qiang, Wang Penglong, Lei Haimin

机构信息

Chinese Academy of Inspection and Quarantine, Beijing 100176, China.

School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100029, China.

出版信息

Se Pu. 2018 Aug 8;36(8):738-744. doi: 10.3724/SP.J.1123.2018.03039.

Abstract

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, 1.7 μm), 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 (>0.99) in their concentration ranges. The limits of detection (LODs) were 0.5 and 1 μg/L, and the limits of quantitation (LOQs) were 2 and 5 μg/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% (=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.

摘要

开发了一种新方法,使用基于离子液体的分散液液微萃取(IL-DLLME)结合超高效液相色谱-串联质谱(UPLC-MS/MS)来测定全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS)从食品接触材料(FCM)中的迁移情况。将FCM样品浸泡在水、10%(v/v)乙醇水溶液和4%(v/v)乙酸溶液这三种食品模拟物中进行迁移试验,然后使用IL-DLLME对迁移液进行萃取和富集。研究了萃取剂类型和体积、涡旋时间、NaCl浓度以及离心速度和时间等关键参数。分析物在Waters ACQUITY UPLC BEH Shield RP18柱(50 mm×2.1 mm,1.7 μm)上分离,用乙腈和水进行梯度洗脱,并采用多反应监测(MRM)在负离子模式下通过电喷雾电离质谱进行定量。实验结果表明,其浓度范围内具有良好的线性关系(>0.99)。PFOA和PFOS的检测限(LOD)分别为0.5和1 μg/L,定量限(LOQ)分别为2和5 μg/L。PFOA和PFOS在三个加标水平下的回收率为86.4%至116.9%,相对标准偏差(RSD)在4.3%至14.4%之间(n = 6)。所提出方法被证明准确、高效、环保,适用于测定PFOA和PFOS从FCM中的迁移情况。

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