干旱区生态环境知识资源中心(Arid): 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

Arid

	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
其他题名	Rapid Screening and Confirmation of Perfluorinated Compounds and Their Precursors in Fish Muscle by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole /Exactive Orbitrap Mass Spectrometry
	郭萌萌 1; 国佼 1; 吴海燕 1; 谭志军 1; 翟毓秀 1; 王智 2; 李兆新 1; 李风铃 1
来源期刊	分析化学
ISSN	0253-3820
出版年	2016
卷号	44 期号:10 页码:1504-1513
中文摘要	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 Exactive Orbitrap MS)的同时定性定量功能,建立了鱼肉中18种全氟化合物(Perfluorinated 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,Oasis PRiME HLB通过式固相萃取柱净化,C_(18)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 Exactive高分辨质谱的Full MS /dd-MS~2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-MS~2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~ 0.50 mug /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。
英文摘要	A method was developed for the rapid screening and confirmation of 18 perfluorinated compounds (PFCs) and 21 precursors in fish muscle by solid phase extraction and liquid chromatography coupled with quadrupole /exactive orbitrap mass spectrometry (LC-Q Exactive Orbitrap MS). In this method,the sample was firstly extracted with acetonitrile-water (90∶ 10,V /V), cleaned-up by solid-phase extraction using Oasis PRiME HLB column. Then,39 target compounds were separated on a BEH C_(18) (2.1 mm100 mm,1.7 mum) column,and the background interference caused by LC system was eliminated by a short C_(18) HPLC column located between the mixer and the auto sampler. In the process of quantification and qualification,a full MS / dd-MS~2 experiment was adopted in mass spectrometry acquisition,accompanied with the full scan MS date for quantification,as well as the date dependent MS~2 product ion spectra for qualification. The mass accuracy error was less than 310~(-6),and the calibration curves were linear well with correlation coefficient over 0.99. The limits of detection ranged from 0.02 to 0.50 mug /kg. The average spiked recoveries for 39 target compounds were between 61.7% and 122.0%,with relative standard derivations (RSDs) from 6.9% to 18.8%. The developed method was successfully applied to the simultaneous determination of 18 PFCs and 21 precursors in fish muscle with satisfactory results.
中文关键词	全氟化合物及其前体物质 ; 鱼肉 ; 四极杆/静电场轨道阱高分辨质谱 ; 固相萃取
英文关键词	Perfluorinated compounds and their precursors Fish muscle Quadrupole /exactive orbitrap mass spectrometry Solid phase extraction
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:5825627
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/234164
作者单位	1.中国水产科学研究院黄海水产研究所, 农业部水产品质量安全检测与评价重点实验室, 青岛, 山东 266071, 中国; 2.青岛市产品质量检验技术研究所,青岛市产品质量监督检验研究院, 青岛, 山东 266061, 中国
推荐引用方式 GB/T 7714	郭萌萌,国佼,吴海燕,等. 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[J],2016,44(10):1504-1513.
APA	郭萌萌.,国佼.,吴海燕.,谭志军.,翟毓秀.,...&李风铃.(2016).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.分析化学,44(10),1504-1513.
MLA	郭萌萌,et al."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".分析化学 44.10(2016):1504-1513.