硫酸磺化—气相色谱/质谱联用法测定土壤中五氯酚及其钠盐

王志强

doi:10.13421/j.cnki.hjwsxzz.2019.01.013

硫酸磺化—气相色谱/质谱联用法测定土壤中五氯酚及其钠盐

王志强

Determination of Pentachlorophenol and its Sodium Salt in Soil by Sulfuric Acid Sulfonate-gas Chromatography/Mass Spectrometry

WANG Zhiqiang

摘要

摘要:
目的建立土壤中五氯酚及其钠盐的硫酸磺化-气相色谱-质谱联用检测方法。
方法土壤中的五氯酚及其钠盐（五氯酚钠）用氢氧化钾涡旋振荡提取，硫酸磺化净化，提取液乙酸酐-吡啶衍生，气相色谱-质谱仪进行测定，2，4，6-三溴酚作内标定量。
结果 PCP在（2.0~40）μg/kg浓度范围内，线性关系良好，相关系数r>0.999，回归方程Y=0.541 42x-0.012 75，加标回收率为85.6%~97.0%，相对标准偏差5.2%~9.0%，检出限0.3 μg/kg。
结论方法快速、灵敏、准确，适用于土壤中五氯酚及其钠盐的分析。

Abstract:
Objectives To establish a sulfuric acid sulfonate-gas chromatography-mass spectrometry to determine pentachlorophenol and its sodium salt in soil.
Methods Pentachlorophenol (PCP) and its sodium salt(NaPCP) in soil were extracted with potassium hydroxide by vortex oscillation, purified by sulfuric acid sulfonation, the extracted solution was derived by using acetic anhydride-pyridine, determined with GC-MS, and quantified with 2, 4, 6-tribromophenol as an internal standard.
Results There was a good linear relationship in the range of (2.0~40) μg/kg PCP, with a correlation coefficient of r>0.999, regression equation Y=0.541 42x-0.012 75, the recovery of standard addition was 85.6%~97.0%, and relative standard deviation was 5.2%~9.0%, detection limit was 0.3 μg/kg.
Conclusions The method was rapid, sensitive and accurate, which was suitable for the analysis of pentachlorophenol and its sodium salt in soil.

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