高效液相色谱-串联质谱法同时测定动物源性食品中全氟辛烷磺酸和全氟辛酸含量

Simultaneous determination of perfluorooctane sulfonate acid and perfluorooctanoic acid in food of animal origin by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  PFOS  PFOA  同位素内标  高效液相色谱-串联质谱

英文关键词:perfluorooctane sulfonate  perfluorooctanoic acid  isotope internal standard  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种同时测定动物源性食品中全氟辛烷磺酸(perfluorooctane sulfonate, PFOS)和全氟辛酸(perfluorooctanoic acid, PFOA)含量的高效液相色谱-串联质谱法的分析方法。方法 从前处理过程和色谱条件两个方面进行优化, 在不使用价格昂贵的同位素内标的情况下提取样品, 流动相为0.05%甲酸-5 mmol/L甲酸铵水溶液和甲醇, 采用多反应监测模式进行分析检测, 外标法定量。结果 PFOS和PFOA含量在0.1~60.0 ng/mL范围内线性良好, 相关系数均大于0.997, PFOS和PFOA定量限分别为0.1 μg/kg、0.01 μg/kg, 样品加标回收率在85%~110%之间, 相对标准偏差均小于10%。该方法适用于检测国家认监委组织的CNCA-23-03(2023)能力验证样品, 能力验证结果为满意。结论 本方法前处理简单, 且不使用价格昂贵的同位素内标, 回收率高, 精密度好, 色谱峰分离效果佳, 适用于动物源性食品中PFOS和PFOA的检测。

英文摘要:

      Objective To establish a high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) in animal-derived foods. Methods The pretreatment process and chromatographic conditions were optimized. Samples were extracted without using expensive isotope internal standard, and the mobile phase was 0.05% formic acid 5 mmol/L ammonium formate aqueous solution and methanol. Multiple reaction monitoring mode was used for analysis and detection, and external standard method was used for quantification. Results The linearity of PFOS and PFOA was good in the range of 0.1?60.0 ng/mL, and the correlation coefficients were both greater than 0.997. The quantitative limits of PFOS and PFOA were 0.1 μg/kg and 0.01 μg/kg, respectively. The recovery rate of samples was between 85% and 110%, and the relative standard deviation was less than 10%. This method was suitable for testing CNCA-23-03(2023) competency verification samples organized by National Certification and Accreditation Administration, and the competency verification result was satisfactory. Conclusion This method has the advantages of simple pretreatment, no expensive isotope internal standard, high recovery rate, good precision and good chromatographic peak separation effect, and is suitable for the detection of PFOS and PFOA in animal-derived foods.