固相萃取-液相色谱-串联质谱法测定食品包装材料中16种全氟烷基类化合物

建立了使用固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)同时检测食品包装材料中16种全氟烷基类化合物(PFAS)的方法。分别对样品前处理方法、质谱条件等进行了比较和优化,样品用甲醇超声提取,经Oasis WAX固相萃取小柱净化后,用Atlantis T3 C₁₈色谱柱分离,以乙腈和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱,多反应监测(MRM)负离子模式扫描,同位素内标法和外标法结合定量。16种PFAS在0.5~20.0 μg/L范围内线性关系良好,相关系数(r²)均大于0.99。加标回收率为68.6%~109.2%,RSD为2.5%~18.1%(n=6)。检出限为0.2~0.5 μg/kg,定量限为0.5~1.0 μg/kg。该方法简便、快速、准确,可用于食品包装材料样品中PFAS的检测。

Determination of 16 perfluorinated alkyl substances in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry

A method for the simultaneous determination of 16 perfluorinated alkyl substances (PFAS) in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was developed. Comparison and optimization of the sample pretreatment methods, mass spectrometry and other conditions were carried out. The samples were ultrasonically extracted with methanol, followed by clean-up using an Oasis WAX SPE column. The analytes were separated on a reversed phase Atlantis T3 C₁₈ column and eluted gradiently with acetonitrile and 5 mmol/L ammonium acetate. The analytes were quantified using isotope internal standard and isotope external standard calibration curve method. The linear calibration curves were obtained in the range of 0.5-20.0 μg/L with the linear relative coefficients more than 0.99. The recoveries were in the range of 68.6%-109.2% and the relative standard deviations (RSDs) were ranged from 2.5% to 18.1% (n=6). The limits of detection (LODs) and the limits of quantification (LOQs) for the PFAS were 0.2-0.5 μg/kg and 0.5-1.0 μg/kg, respectively. This method is simple, rapid, accurate and can be used in the determination of PFAS in food packaging materials.