Eberlin Marcos Nogueira, Cesar da Silva Rogério
ThoMSon Mass Spectrometry Laboratory, Institute of Chemistry, State University of Campinas, 13084-971 Campinas, SP, Brazil.
Anal Chim Acta. 2008 Jul 14;620(1-2):97-102. doi: 10.1016/j.aca.2008.05.033. Epub 2008 May 22.
Solid phase microextraction (SPME) of chlorophenols [2-chlorophenol (2CP), 2,4-dichlorophenol (24CP), 4-chloro-3-methylphenol (43CP), 2,4,6-tri-chlorophenol (246CP) and pentachlorophenol (PCP)] followed by direct mass spectrometric analysis has been performed by fiber introduction mass spectrometry (FIMS). Two SPME fibers (65 microm PDMS/DVB and 85 microm PA fibers) were tested, and FIMS was performed via selective ion monitoring (SIM). The extractions were evaluated at 10% ionic strength and pH 1. Best extraction times were determined for both fibers. Limits of detection (LOD) and limits of quantification (LOQ) for both fibers were in the low microg L(-1) range. Coefficients of correlation for the analytical curves showed linear responses and mineral water and river water samples spiked with 50 microg L(-1) presented high recoveries. FIMS, as compared to current EPA methods, is demonstrated to allow faster and simpler (elimination of pre-separation or derivatization steps) analysis of chlorophenols in water with the required sensitivity.
采用光纤引入质谱法(FIMS)对氯酚类物质[2-氯酚(2CP)、2,4-二氯酚(24CP)、4-氯-3-甲基酚(43CP)、2,4,6-三氯酚(246CP)和五氯酚(PCP)]进行固相微萃取(SPME),随后进行直接质谱分析。测试了两种SPME纤维(65微米聚二甲基硅氧烷/二乙烯基苯和85微米聚丙烯酸酯纤维),并通过选择性离子监测(SIM)进行FIMS分析。在10%离子强度和pH值为1的条件下对萃取效果进行评估。确定了两种纤维的最佳萃取时间。两种纤维的检测限(LOD)和定量限(LOQ)均在低微克/升(μg L⁻¹)范围内。分析曲线的相关系数显示出线性响应,加标浓度为50微克/升(μg L⁻¹)的矿泉水和河水样品具有较高的回收率。与现行美国环保署方法相比,FIMS能够在所需灵敏度下更快、更简单地(无需预分离或衍生化步骤)分析水中的氯酚类物质。