超高效液相色谱-高分辨质谱法同时测定鱼肉中16种全氟烷基化合物  

Simultaneous Determination of 16 Kinds of PerfluoroalkylSubstances in Fish Muscle by Ultra High Performance LiquidChromatography-High Resolution Mass Spectrometry

作　　者：涂祥婷 杨鸿波 郭峰[2] 曾士宜 滕春丽 孙晓红 何锦林 林绍霞 TU Xiang-Ting;YANG Hong-Bo;GUO Feng;ZENG Shi-Yi;TENG Chun-Li;SUN Xiao-Hong;HE Jin-Lin;LIN Shao-Xia(The Key Laboratory of Environmental Pollution Monitoring and Disease Control,Ministry of Education,School of Public Health,Guizhou Medical University,Guiyang 550025,China;Key Laboratory of Eco-Geochemistry,Ministry of Natural Resources,National Research Center for Geoanalysis,Beijing 100037,China;Guizhou Academy of Testing and Analysis,Guiyang 550016,China)

机构地区：[1]贵州医科大学公共卫生学院,环境污染与疾病监控教育部重点实验室,贵阳550025 [2]国家地质实验测试中心,自然资源部生态地球化学重点实验室,北京100037 [3]贵州省分析测试研究院,贵阳550016

出　　处：《分析化学》2021年第4期528-537,共10页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21966011,21976044);中央引导地方科技发展专项资金项目(No.黔科中引地[2016]4001);中央级公益性科研院所基本科研业务费项目(No.CSJ201906)资助。

摘　　要：建立了快速滤过型净化(Multi-plug filtration cleanup,m-PFC)-超高效液相色谱-四极杆-静电场离子轨道阱高分辨质谱法同时测定鱼肉中16种全氟烷基化合物(Perfluorinated alkylated substances,PFASs)。样品经1%甲酸-乙腈溶液超声提取,通过式m-PFC固相萃取柱净化,氮吹浓缩至1 mL后,以AcquityWaters BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm)分离,甲醇-5 mmol/L乙酸铵溶液进行梯度洗脱。质谱采用Full MS/dd-MS 2扫描模式,正离子和负离子切换扫描,采用内标法进行定量分析。在最佳的分析条件下,16种目标物在13 min内均可实现良好分离,各物质的精确质量数偏差均小于2.83×10^(-6),在0.10~20.0μg/L浓度范围内,各化合物线性关系良好,相关系数(R^(2))均大于0.990,方法的检出限为0.015~0.05μg/kg。在0.50、2.0和5.0μg/kg的基质加标水平下,平均回收率为70.7%~110.1%,相对标准偏差(Relative standard deviations,RSDs)为0.5%~12.8%。将本方法应用于25个野生鱼样品的快速分析,共检出10种PFASs,其中全氟辛酸(Perfluorooctane sulfonate,PFOS)为主要污染物。本方法操作简单、快速、准确度高、灵敏度高,适用于鱼肉中16种PFASs的快速检测。A method for determination of 16 kinds of perfluoroalkyl substances in fish muscle by multi-plug filtration cleanup(m-PFC)combined with ulrahigh performance liquid chromatography-Q-extractive orbitrap high resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS)was established.The samples were ultrasonically extracted by 1%formic acid-acetonitrile,purified by solid phase extraction using m-PFC column and concentrated to 1 mL under nitrogen.The analytes were separated on an Acquity Waters BEH C 18(50 mm×2.1 mm,1.7μm)column,and gradient eluted with 5 mmol/L ammonium acetate and methanol.The MS acquisition mode was Full MS/dd-MS^( 2) in both negative and positive ionization mode,and the internal standard method was used for quantification.Under the best analytical conditions,a total of 16 target compounds were well separated within 13 min,and the accurate mass deviation of each substance was less than 2.83×10^(-6).A good linearity was obtained in the concentration ranges of 0.10-20.0μg/L with correlation coefficients of greater than 0.990.The MDLs ranged from 0.015μg/kg to 0.05μg/kg.The average recoveries of 16 kinds of PFASs spiked at 0.50,2.0 and 5.0μg/kg were 70.7%-110.1%and the relative standard deviations(RSDs)were 0.5%-12.8%.The established method was successfully applied to the rapid detection of 25 wild fish samples.Ten PFASs were detected,in which PFOS were the predominant pollutant.The method was simple,rapid,accurate and sensitive,and suitable for the rapid detection of 16 kinds of PFASs in fish muscle.

关 键 词：四极杆-静电场离子轨道阱高分辨质谱 快速滤过型净化 鱼肉 全氟烷基化合物 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]