Sin-QuEChERS净化技术结合液相色谱-串联质谱法检测大棚蔬菜中13种全氟烷基酸

Determination of 13 kinds of perfluoroalkyl acids in greenhouse vegetables by Sin-QuEChERS purification technology and liquid chromatography-tandem mass spectrometry

中文关键词:  全氟烷基酸  Sin-QuEChERS  液相色谱-串联质谱法  大棚蔬菜

英文关键词:perfluoroalkyl acids  Sin-QuEChERS  liquid chromatography-tandem mass spectrometry  greenhouse vegetable

中文摘要:

      目的 建立基于Sin-QuEChERS净化技术结合液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速检测大棚蔬菜中13种全氟烷基酸(perfluoroalkyl acids, PFAAs)的分析方法。方法 采用0.5%甲酸-乙腈提取目标物, 无水MgSO4和NaCl盐析脱水, 随后采用封装了100 mg N-丙基乙二胺(primary secondary amine, PSA)、80 mg封端十八烷基硅胶(C18)、50 mg石墨化碳黑(graphitized carbon black, GCB)、50 mg多壁碳纳米管(multi-wall carbon nanotubes, MWCNTs)净化粉和800 mg无水MgSO4的Sin-QuEChERS通过式快速净化管净化除去基质干扰物, 浓缩定容后采用LC-MS/MS分析, 并采用同位素内标辅助定量。结果 13种物质的标准曲线线性相关系数均大于等于0.997, 检出限为0.004~0.008 μg/kg, 定量限为0.009~0.023 μg/kg; 多种蔬菜基质中的加标回收率在75.4%~104.1%之间, 相对标准偏差不超过8.1%, 满足痕量分析要求; 基质效应干扰多数可忽略, 表明了良好的净化效果及方法适用性。与其他方法相比, 本方法净化操作时间缩短一半以上, 显著提高了前处理效率。结论 与现有分析方法相比, 本方法具有快速、操作简便、重复性和准确性优、基质适用性强等特点, 适宜常见大棚蔬菜中PFAAs大规模检测分析, 具有一定实际意义。

英文摘要:

      Objective To establish a rapid analysis method for the determination of 13 kinds of perfluoroalkyl acids (PFAAs) in greenhouse vegetables based on Sin-QuEChERS purification technology and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Targets were extracted by acetonitrile added with 0.5% formic acid, following salting out and dehydration by anhydrous MgSO4 and NaCl, then a Sin-QuEChERS purification column filling with 100 mg primary secondary amine (PSA), 80 mg C18, 50 mg graphitized carbon black (GCB), 50 mg multi-wall carbon nanotubes (MWCNTs) and 800 mg anhydrous MgSO4 was employed to remove the interferent substances, and analyzed by LC-MS/MS after concentrated and redissolved at last, while isotope internal standards were used for auxiliary quantitative analysis. Results The linear equation correlation coefficients of 13 kinds of substances were all greater than or equal to 0.997, while the limits of detection and the limits of quantitation were in the range of 0.004?0.008 μg/kg and 0.009?0.023 μg/kg, respectively. The recoveries for various kinds of vegetable matrix were in the range of 75.4%?104.1% and the relative standard deviations were no more than 8.1%, meeting the requirement of trace analysis. Matrix effect evaluation showed that the substances were slightly affected, reflecting satisfactory purification process of this method. Compared with other methods, the time of purification process had been decreased by more than half in this method, leading to significant improvement of pretreatment efficiency. Conclusion Compared with existing analytical methods, this method has advantages of simple operation, time consuming, excellent repeatability and accuracy, and strong matrix applicability, which is suitable for the efficient analysis of PFAAs in greenhouse vegetables with large scale, and has certain practical significance.