建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂蜜中2 0种全氟烷基化合物( PFASs)含量的分析 方法.采用改进的QuEChERS方法对样品进行前处理,用含1. 5% (v/v )甲酸的乙腈溶液振荡提取, C,8和况-丙基 乙二胺( PSA)吸附剂净化,Atlantis T3 C18色谱柱(150mm×2. 1 mm,3 pm)分离,以含5 mmol/L 乙酸铵的甲醇溶 液和5 mmol/L 乙酸铵溶液为流动相进行梯度洗脱.在电喷雾离子( ESI)源负离子模式下以多反应监测( MRM) 扫描,采用同位素内标法进行定量分析.结果表明,20种 PFASs在16 m in内即可完成分离,在0.2-10 pg/L范围 内线性关系良好,相关系数(r )均大于0.99;检出限( LOD, S/况= 3 )和定量限( LOQ, S/况=10)分别为0.04-0. 10 pg/kg 和 0.10-0.20 pg/kg.在 0.1、0.5、1.0 和 2.0 pg/kg 加标水平下,20 种 PFASs 的加标回收率为 72.6%- 113. 0%, RSD为0. 4% -15. 9% (w = 6 ).该法快速、高效、准确,适用于蜂蜜样品中2 0种 PFASs的同时检测.
A sensitive method for simultaneous determination of 20 perfluorinated alkyl sub-stances (PFASs) in honey was developed by QuEChERS-high performance liquid chromatogra-phy-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted by acetonitrile with 1. 5% (v/v ) formic acid,and purified by Cm and W-propylethylenediamine (PSA) adsor-bents. The separation of the 20 PFASs was performed on an Atlantis T3 C18 column using gradi-ent elution with methanol containing 5 mmo^L ammonium acetate and 5 mmol/L ammonium acetate as mobile phases within 16 min. The PFASs were analyzed under the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-). Under the optimal con-ditions, the isotope internal standard method was used to quantify the contents of the 20 PFASs. The calibration curves were acquired in the concentration range of 0.2-10 pg/L with correlation coefficients (r ) greater than 0. 99. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.04 to 0. 10 pg/kg and 0. 10 to 0.20 pg/kg, respectively. The recoveries of the 20 PFASs spiked in blank honey samples were between 72. 6% and 113.0% with relative standard derivations ( RSDs) of 0.4% -15.9% ( n = 6). The developed method is rapid,efficient and accurate,and suitable for the simultaneous analysis of the 20 PFASs in honey samples.