论文部分内容阅读
[目的]研究运用超高效液相色谱-三重四极杆串联质谱仪测定植物样品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的可行性。[方法]建立了一种SPE净化,超高效液相色谱-三重四极杆串联质谱仪UPLC/MS/MS方法测定植物(绿萝)根、茎和叶中PFOS和PFOA残留量,并优化了质谱条件和前处理方式,保留时间分别为2.26和2.17 min。[结果]采用碳酸钠(Na2CO3)、四丁基硫酸氢铵(TBAHS)、甲基叔丁基醚(MTBE)作为提取试剂,HLB小柱净化后PFOS在绿萝根、茎、叶中的加标回收率为46.53%~77.35%,变异系数为5.63%~18.52%;PFOA在绿萝根、茎、叶中的加标回收率为59.01%~100.46%,变异系数为2.85%~30.06%,检出限分别为26.90×10-4和3.09×10-4ng,相关系数均大于0.998。[结论]超高效液相色谱-三重四极杆串联质谱仪测定植物样品中PFOS和PFOA满足化合物残留分析要求。
[Objective] The research aimed to study the feasibility of determination of PFOS and PFOA in plant samples by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry. [Method] A UPLC / MS / MS method was developed for the determination of PFOS and PFOA residues in roots, stems and leaves of plant (green radish) by SPE purification and ultra performance liquid chromatography-triple quadrupole mass spectrometry. Conditions and pretreatment methods, retention time was 2.26 and 2.17 min. [Result] The effects of sodium bicarbonate (Na2CO3), tetrabutylammonium hydrogen sulfate (TBAHS) and methyl tert-butyl ether (MTBE) on the extraction of PFOS in the root, The recoveries ranged from 46.53% to 77.35%, and the coefficients of variation ranged from 5.63% to 18.52%. The spiked recoveries of PFOA in roots, stems and leaves were 59.01% ~ 100.46%, and the coefficients of variation were 2.85% ~ 30.06% The limits were 26.90 × 10-4 and 3.09 × 10-4ng, the correlation coefficients were all greater than 0.998. [Conclusion] The determination of PFOS and PFOA in plant samples by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry met the requirements of compound residue analysis.