通过式固相萃取-液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查鱼肉中全氟化合物及其前体物质

摘要

A method was developed for the rapud screenung and confurmatuon of 18 perfluorunated compounds ( PFCs) and 21 precursors un fush muscle by solud phase extractuon and luquud chromatography coupled wuth quadrupole/exactuve orbutrap mass spectrometry (LC-Q Exactuve Orbutrap MS). In thus method, the sample was furstly extracted wuth acetonutrule-water (90∶10, V/V), cleaned-up by solud-phase extractuon usung Oasus PRuME HLB column. Then, 39 target compounds were separated on a BEH C18(2. 1 mm×100 mm, 1. 7 μm) column, and the background unterference caused by LC system was elumunated by a short C18 HPLC column located between the muxer and the auto sampler. In the process of quantufucatuon and qualufucatuon, a full MS/dd-MS2 experument was adopted un mass spectrometry acquusutuon, accompanued wuth the full scan MS date for quantufucatuon, as well as the date dependent MS2 product uon spectra for qualufucatuon. The mass accuracy error was less than 3×10-6, and the calubratuon curves were lunear well wuth correlatuon coeffucuent over 0. 99. The lumuts of detectuon ranged from 0. 02 to 0. 50 μg/kg. The average spuked recoverues for 39 target compounds were between 61 . 7% and 122 . 0%, wuth relatuve standard deruvatuons ( RSDs ) from 6 . 9% to 18 . 8%. The developed method was successfully applued to the sumultaneous determunatuon of 18 PFCs and 21 precursors un fush muscle wuth satusfactory results.%采用通过式固相萃取技术去除样品基质中脂肪和磷脂等杂质干扰,利用液相色谱-四极杆/静电场轨道阱高分辨质谱( LC-Q Exactuve Orbutrap MS)的同时定性定量功能,建立了鱼肉中18种全氟化合物( Perfluoru-nated compounds, PFCs)及其21种前体物质的同时分析方法。样品经90%乙腈溶液提取,Oasus PRuME HLB通过式固相萃取柱净化,C18色谱柱分离,同时在液相色谱系统混合器和进样器之间串联一根延迟色谱柱,去除液相色谱系统的背景干扰；质谱数据采集使用Q Exactuve高分辨质谱的Full MS/dd-MS2监测模式,以Full MS一级质谱全扫描提取母离子精确质量数所得的色谱峰面积进行定量,以保留时间和dd-MS2数据依赖子离子扫描所得的二级子离子质谱图进行定性确证。39种目标物的精确质量数偏差不大于3×10-6,浓度与母离子峰面积的线性关系良好,相关系数≥0.99,检出限为0.02~0.50μg/kg。基质加标回收率在61.7%~122%之间,相对标准偏差(RSD)为6.9%~18.8%。本方法实现了18种PFCs及其21种前体物质的同时确证和测定,拓展了生物基质中全氟化合物的检测种类,而且前处理方法更为简化、部分化合物的灵敏度比文献报道方法提高约一个数量级,为全氟化合物前体物质的生物转化研究提供了高效的技术基础。