高效液相色谱-串联质谱法测定蜂蜜中20种全氟烷基化合物  

Determination of 20 perfluorinated alkyl substances in honey by high performance liquid chromatography-tandem mass spectrometry

作　　者：李帅[1] 陈辉[2] 金铃和 彭涛[2] 范春林[2] 王明林[1] 

机构地区：[1]山东农业大学食品科学与工程学院,山东泰安271018 [2]中国检验检疫科学研究院,北京100176

出　　处：《色谱》2017年第5期495-501,共7页Chinese Journal of Chromatography

基　　金：国家科技基础性工作专项(2013FY113100)~~

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂蜜中20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_(18)和N-丙基乙二胺(PSA)吸附剂净化,Atlantis T3 C_(18)色谱柱(150 mm×2.1 mm,3μm)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 min内即可完成分离,在0.2~10μg/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/N=3)和定量限(LOQ,S/N=10)分别为0.04~0.10μg/kg和0.10~0.20μg/kg。在0.1、0.5、1.0和2.0μg/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%(n=6)。该法快速、高效、准确,适用于蜂蜜样品中20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.

关 键 词：高效液相色谱-串联质谱 QuEChERS方法 全氟烷基化合物 蜂蜜 

分 类 号：O658[理学—分析化学]