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应用搅拌棒吸附萃取富集及热解吸进样与气相色谱-质谱相结合测定了水样中3种烷基酚(即正辛基酚、叔辛基酚和正壬基酚)的含量。将水样预先用盐酸调节其酸度至pH 3,分取10.00mL置于顶空瓶中,放入搅拌棒进行吸附萃取。取出搅拌棒,置于热脱附管上解吸并通过程序升温进样系统进样,用DB-5MS柱进行色谱分离。质谱分析条件:电子轰击正离子源,全扫描模式(定性分析)和选择离子扫描模式(定量分析)。3种烷基酚的质量浓度均在5~200ng·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在1.2~2.5ng·L-1之间。以实际水样为基体进行加标回收试验,测得回收率在95.0%~118%之间,测定值的相对标准偏差(n=5)在0.90%~10%之间。
The contents of three kinds of alkylphenols (n-octylphenol, t-octylphenol and n-nonylphenol) in water sample were determined by the combination of stir bar absorption and enrichment, thermal desorption and gas chromatography-mass spectrometry. The water sample was adjusted with hydrochloric acid before its acidity to pH 3, 10.00mL points were placed in a headspace bottle, placed in a stirring rod adsorption extraction. The stir bar was removed and placed on a desorption tube and desorbed through a programmed temperature injection system and chromatographed on a DB-5MS column. Mass Spectrometry Conditions: Electron Impact Positive Ion Source, Full Scan Mode (Qualitative Analysis), and Selected Ion Scan Mode (Quantitative Analysis). The concentration of 3 alkylphenols in the range of 5 ~ 200ng · L-1 showed a linear relationship with the peak area. The detection limit (3S / N) of the three alkylphenols was between 1.2 and 2.5 ng · L-1. The actual water samples were collected for spike recovery test. The recoveries were between 95.0% and 118%. The relative standard deviations (n = 5) of the measured values ranged from 0.90% to 10%.