色谱

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Tenax采样管富集气相色谱-质谱法测定空气中的痕量酚类化合物

杨丽莉,胡恩宇,母应锋,纪英   

  1. Nanjing Environment Monitoring Center, Nanjing 210013, China
  • 收稿日期:2006-05-29 修回日期:2006-07-21 出版日期:2007-01-30 发布日期:1986-03-25
  • 通讯作者: 杨丽莉

Determination of Trace Phenol Compounds Using Gas Chromatography-Mass Spectrometry Coupled with Tenax Adsorption Tube for Enrichment of Air Samples

YANG Lili, HU Enyu, MU Yingfeng, JI Ying   

  1. Nanjing Environment Monitoring Center, Nanjing 210013, China
  • Received:2006-05-29 Revised:2006-07-21 Online:2007-01-30 Published:1986-03-25
  • Contact: YANG Lili

摘要: 建立了Tenax采样管富集气相色谱-质谱测定空气中痕量酚类化合物的方法。用Tenax采样管吸附环境空气中的痕量酚类化合物,用甲醇淋洗解吸酚类化合物,洗脱液加入萘-D8作为内标,利用气相色谱-选择离子监测质谱(GC-MS/SIM)进行检测,内标法定量。该方法定性、定量准确,线性响应良好,回归曲线的线性相关系数均大于0.999,平均回收率为92.4%~102%,测定干扰小,检测灵敏度高,按采样10 L计算,空气中最低检测浓度可达0.001 mg/m3。用于实际样品测定,完全能满足环境空气中痕量酚类化合物监测的要求。

关键词: Tenax采样管, 酚类化合物, 空气样品 , 气相色谱-质谱法

Abstract: A novel determination method for trace of seven phenol compounds in air samples has been established. They were collected with Tenax adsorption tube (180 mm×60 mm glass tube packed with 150 mg Tenax (4060 mesh)) and desorbed with methanol. Five microlitres of naphthalene-D8 (internal standard) solution was added to the eluate. One microlitre of the mixture solution was injected into an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) and determined by gas chromatography-mass spectrometry with selected ion monitoring (GC-MS/SIM). The selected ions were m/z 94, 95, 66, 108, 107, 77, 90, 122, 121, 107 and 136. The quantitative ions, m/z 94 for phenol, m/z 108 for cresol, m/z 122 for xylenol and m/z 136 for internal standard, were selected. The average recoveries of phenol compounds (spiked at the levels of 0.25, 1.00, 5.00 μg) ranged from 92.4% to 102% and the relative standard deviations were less than 4.8%. When the air sample volume was 10 L, the detection limits were less than 0.001 mg/m3. Good linearities were observed in the range from 0.05 to 20.0 mg/L. The method is simple, fast, sensitive and accurate for the determination of phenol compounds in air samples.

Key words: air sample , gas chromatography-mass spectrometry (GC-MS), phenol compounds, Tenax adsorption tube