高效液相色谱-串联质谱法测定婴幼儿米粉中12种全氟烷基化合物

Determination of 12 perfluorinated compounds in rice powder for infants and young children by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱  全氟烷基化合物  婴幼儿米粉

英文关键词:high performance liquid chromatography-tandem mass spectrometry  perfluorinated compounds  rice powder for infants and young children

中文摘要:

      目的 建立了高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定婴幼儿辅食米粉中12种全氟烷基化合物(perfluorinated compounds, PFCs)的方法。方法 样品经酸化乙腈提取, 加入乙二胺-N-丙基硅烷(ethylenediamine-n-propylsilane, PSA), C18, 石墨化碳黑(Graphitized carbon black, GCB)3种吸附剂后, 涡旋振荡对样品进行净化。利用C18反相色谱柱对婴幼儿辅食米粉中12种PFCs进行分离, 负离子模式电喷雾电离, 配合多级反应离子扫描(multiple reaction monitoring, MRM)定性定量分析目标化合物。考察了流动相和色谱柱对分离检测的影响, 优化了主要影响因素和实验条件, 在条件优化过程中采用外标法进行定量分析。结果 12种PFCs标准曲线的线性相关系数大于0.995, 检出限为0.07~0.15 μg/kg, 在0.2、0.5、1.0 μg/kg加标水平下, 样品的加标回收率为68.8%~115.4%, 相对标准偏差(relative standard deviation, RSD)为1.25%~15.6% (n=6)。结论 该方法操作简便, 分离效果好, 检出限低, 适用于婴幼儿辅食米粉中PFCs的检测。

英文摘要:

      Objective To establish a method of determination of 12 perfluorinated compounds (PFCs) in infant food supplements by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with acidified acetonitrile, and after adding three kinds of adsorbents, ethylenediamine-n-propylsilane (PSA), C18, and graphitized carbon black (GCB), the sample was vortexed and purified. The 12 PFCs in infant food supplement rice flour were separated by C18 reversed-phase chromatography column, negative ion mode electrospray ionization, and multi-stage reactive ion scanning (MRM) qualitative and quantitative analysis of target compounds. The effects of mobile phase and column on separation detection were investigated. The main influencing factors and experimental conditions were optimized. The external standard method was used for quantitative analysis in the condition optimization process. Results The linear correlation coefficient of the 12 PFCs standard curves was more than 0.995, and the detection limit was 0.07?0.15 μg/kg. At the spiked levels of 0.2, 0.5, 1.0 μg/kg, the spiked recoveries of the samples were 68.8%?115.4%. The relative standard deviation (RSD) was between 1.25% and 15.6% (n=6). Conclusion The method is simple in operation, good in separation effect and low in detection limit, which is suitable for detecting PFCs in infant food supplement rice flour.