PDF《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》

2018 年8月Vol.

36 No.8 August

2018 Chinese Journal of Chromatography 738~744 研究论文 DOI: 10.3724/ SP.J.1123.2018.03039 ?收稿日期:2018?03?31 # 共同第一作者. ?通讯联系人.Tel:(010)53897463,E?mail:maqiang@ caiq.gov.cn(马强);

Tel:(010)53897466,E?mail:baih@ caiq.gov.cn(白桦). 基金项目:国家重点研发计划(2016YFF0203701). Foundation item: National Key Research &

Development Program of China (No. 2016YFF0203701). 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 闫萌萌1,2# , 陈萌1,2# , 孟宪双1 , 郭项雨1 , 白桦1? , 马强1? , 王鹏龙2 , 雷海民2 (1. 中国检验检疫科学研究院, 北京 100176;

2. 北京中医药大学中药学院, 北京 100029) 摘要: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?

7 μm), 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(r2 >

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. 关键词:离子液体;

分散液液微萃取;

超高效液相色谱?串联质谱;

全氟辛酸;

全氟辛烷磺酸;

食品接触材料;

食品模拟物 中图分类号:O658 文献标识码:A 文章编号:1000?8713(2018)08?0738?07 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 YAN Mengmeng1,2# , CHEN Meng1,2# , MENG Xianshuang1 , GUO Xiangyu1 , BAI Hua1? , MA Qiang1? , WANG Penglong2 , LEI Haimin2 (1. Chinese Academy of Inspection and Quarantine, Beijing 100176, China;

2. School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100029, China) 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 第8期闫萌萌,等: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 investigated. The analytes were separated on a Waters ACQUITY UPLC BEH Shield RP18 col? umn (50 mm*2?