Maggi Luana, Zalacain Amaya, Mazzoleni Valeria, Alonso Gonzalo L, Salinas M Rosario
Istituto di Enologia e Ingegneria agro-alimentare, Università Católica del Sacro Cuore, 29100 Piacenza, Italy.
Talanta. 2008 May 15;75(3):753-9. doi: 10.1016/j.talanta.2007.12.013. Epub 2007 Dec 23.
Solid-phase microextraction by immersion (IS-SPME) and headspace mode (HS-SPME), together with stir bar sorptive extraction (SBSE), have been assayed in combination with gas chromatography-ion trap tandem mass spectrometry (MS/MS) for analysing 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, 2,4,6-tribromophenol, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole and 2,4,6-tribromoanisole in different liquid matrices. Once, the optimization of MS/MS fragmentation analysis was carried out, sample enrichment was performed using the three mentioned extraction methods, and comparison through the determination of linearity, and LOD and LOQs were carried out. SBSE and IS-SPME methods described enabled us to determine the target compounds at ng/l levels, concentrations lower than their olfactory threshold, which is not the case of HS-SPME. SBSE showed a higher concentration capability than both SPME techniques, especially when compared to the HS-SPME mode. Thus, SBSE should be the definitive technique to analyse halophenols and haloanisoles in aqueous matrices. SBSE has been also applied to nine aqueous matrices as different as tap water, wines or commercial lemon juice extract.
已将浸入式固相微萃取(IS-SPME)和顶空模式(HS-SPME)以及搅拌棒吸附萃取(SBSE)与气相色谱-离子阱串联质谱(MS/MS)结合起来,用于分析不同液体基质中的2,4,6-三氯苯酚、2,3,4,6-四氯苯酚、2,4,6-三溴苯酚、2,4,6-三氯苯甲醚、2,3,4,6-四氯苯甲醚和2,4,6-三溴苯甲醚。一旦完成了MS/MS碎片分析的优化,便使用上述三种萃取方法进行样品富集,并通过测定线性、检测限(LOD)和定量限(LOQ)进行比较。所描述的SBSE和IS-SPME方法使我们能够测定纳克/升水平的目标化合物,其浓度低于它们的嗅觉阈值,而HS-SPME则不然。SBSE显示出比两种SPME技术更高的浓缩能力,尤其是与HS-SPME模式相比时。因此,SBSE应该是分析水性基质中卤代酚和卤代苯甲醚的决定性技术。SBSE还已应用于九种不同的水性基质,如自来水、葡萄酒或市售柠檬汁提取物。