高级检索

    高效液相色谱-串联质谱法同时测定空气中10种酚类化合物的含量

    Simultaneous Determination of 10 Phenolic Compounds in Air by High Performance Liquid Chromatography-Tandem Mass Spectrometry

    • 摘要: 提出了高效液相色谱-串联质谱法同时测定空气中苯酚、4-硝基酚、3-甲酚、2-氯酚、2,4-二甲酚、2,4-二氯酚、2,4,6-三氯酚、五氯酚、1-萘酚、2-萘酚等10种酚类化合物含量的方法。用XAD-7采样管采样,用甲醇洗脱;收集2.0 mL洗脱液,分取0.5 mL,再用水定容至1.0 mL,过0.22 μm滤膜。以Kinetex C18色谱柱为固定相,以不同体积比的甲醇-水的混合溶液为流动相进行梯度洗脱。分离后的酚类化合物经大气压化学电离源电离,多反应监测模式检测,外标法定量。结果表明:10种酚类化合物标准曲线的线性范围均为10~1 000 μg·L-1,检出限(3.143s)为0.2~1.7 μg·m-3;对空白样品进行3个浓度水平的加标回收试验,回收率为69.3%~102%,测定值的相对标准偏差(n=6)为1.1%~9.6%;方法用于10个实际空气样品分析,其中有3个样品检出苯酚,质量浓度为23.3~40.2 μg·m-3

       

      Abstract: A method for the simultaneous determination of 10 phenolic compounds, including phenol, 4-nitrophenol, 3-cresol, 2-chlorophenol, 2, 4-xylenol, 2, 4-dichlorophenol, 2, 4, 6-trichlorophenol, pentachlorophenol, 1-naphthol and 2-naphthol in air by high performance liquid chromatography-tandem mass spectrometry was proposed. XAD-7 sampling tube was used for sampling, and methanol was used for elution. The eluent (2.0 mL) was collected, and an aliquot (0.5 mL) was taken. Then its volume was made up to 1.0 mL with water, and the mixed solution was filtered by 0.22 μm filter membrane. Kinetex C18 chromatographic column was used as the stationary phase, and the mixed solutions composed of methanol and water at different volume ratios was used as the mobile phase for gradient elution. The separated phenolic compounds were ionized by atmospheric pressure chemical ionization source, detected by multi-reaction monitoring mode, and quantified by external standard method. It was shown that the linear ranges of the standard curves for 10 phenolic compounds were 10-1 000 μg·L-1, with detection limits (3.143s) in the range of 0.2-1.7 μg·m-3. Test for recovery was made on the blank sample at 3 concentration levels, giving results in the range of 69.3%-102%, and RSDs of the determined values (n=6) ranged from 1.1% to 9.6%. The method was applied to analyze 10 actual air samples, among which 3 samples detected phenol with the mass concentrations in the range of 23.3-40.2 μg·m-3.

       

    /

    返回文章
    返回