杂质延迟-液相色谱-四极杆/离子阱复合质谱测定水产加工食品中23种全氟烷基化合物  

Simultaneous Identification and Detection of 23 Perfluorinated Alkyl Substances in Processed Aquatic Products by Impurity Delay Using Liquid Chromatography Coupled with Quadrupole/Linear Ion Trap Mass Spectrometry

作　　者：郭萌萌[1,2] 吴海燕[1,2] 卢立娜[1,2] 谭志军[1,2] 翟毓秀[1,2] 赵春霞[1,2] 付树林[1,2] 李兆新[1,2] 

机构地区：[1]农业部水产品质量安全检测与评价重点实验室,中国水产科学研究院黄海水产研究所,青岛266071 [2]国家水产品质量监督检验中心,青岛266071

出　　处：《分析化学》2015年第8期1105-1112,共8页Chinese Journal of Analytical Chemistry

基　　金：国家科技基础性工作专项(No.2014FY230100)资助项目~~

摘　　要：采用杂质延迟法去除液相系统中的背景干扰,利用液相色谱-四极杆/线性离子阱复合质谱（LC-MS/MS-QTRAP）的同时定性定量功能,建立了水产加工食品中23种全氟烷基化合物（Perfluorinated alkyl substances,PFASs）的定性确证和定量测定方法。样品经酸化乙腈提取,C18填料和石墨化碳黑（GCB）分散固相萃取净化,C18色谱柱分离,甲醇和5 mmol/L乙酸铵溶液梯度洗脱;在液相系统混合器和进样器之间串联一根延迟色谱柱,去除液相系统的背景干扰;质谱采集使用MS/MS-QTRAP独有的多反应监测（MRM）-信息依赖性采集（IDA）-增强子离子扫描（EPI）模式;同位素内标定量,在线EPI谱库定性确证。23种目标物在各自相应浓度范围内线性良好,相关系数不低于0.995,定量限为0.02~0.1μg/kg。基质加标回收率在67.5%~116.4%之间,相对标准偏差（RSD）为5.2%~14.7%。本方法有效控制了液相系统的背景干扰,一次进样即可完成23种PFASs的确证和测定,适用于水产加工食品中PFASs的监控分析。A comprehensive method for the simultaneous identification and detection of 23 perfluorinated alkyl substances （PFASs） in processed aquatic products by impurity delay was developed using liquid chromatography coupled with quadrupole/linear ion trap tandem mass spectrometry （LC-Q/Trap-MS）. The sample was extracted with acidified acetonitrile, cleaned-up by dispersive solid phase extraction using C18 and graphitized carbon blacks （GCB）. The separation of 23 PFASs was performed on a Kinetex XB-C18（ 100 mmx 2.1 mm,2.6 μm） column using gradient elution of 5 mmol/L ammonium acetate and methanol as mobile phase. And a short Cls HPLC column was inserted between the mixer and the autosample, which delayed compounds coming from the LC system. A scheduled multiple reaction monitoring （MRM） in negative mode as survey scan and an enhanced product ion （EPI） scan as dependent scan in an information-dependent acquisition （IDA） experiment were adopted in mass spectrometry acquisition. On-line lab-buih MS/MS library and the isotope internal standards were employed for the identification and quantification. The calibration curves for the detection of 23 PFASs were linear well with correlation coefficient over 0. 995. The limits of quantification for all analytes were ranged from 0.02μg/kg to 0. 1μg/kg. The average spiked recoveries for 23 PFASs were between 67.5% and 116.4%, with relative standard deviations （RSDs） from 5.2% to 14.7%. The background coming from the part of LC was controlled well by the impurity delay. The proposed method can be used to identify and detect the 23 PFASs in a single run, and also suitable for the analysis of processed aquatic product samples.

关 键 词：全氟烷基化合物 水产加工食品 杂质延迟法 液相色谱-三重四极杆/线性离子阱复合质谱 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]