摘要
目的建立农田土壤中五氯酚(PCP)的固相萃取-气相色谱-质谱(SPE-GC-MS)检测方法。方法土壤中的PCP用乙酸乙酯-正己烷(1∶1,V/V)在酸性条件下提取,萃取液经SLC固相萃取柱净化,用乙腈洗脱,乙酸酐衍生,采用DB-5MS毛细管色谱柱分离,用GC-MS法测定,2,4-二溴酚作内标定量。结果 PCP的浓度为2.0μg/kg^40μg/kg时,线性关系良好,回归方程为y=0.056 2x+0.001 4,相关系数为0.999 6。土壤中加标浓度为2.5μg/kg^20.0μg/kg时,平均回收率为85.6%~97.0%,相对标准偏差为5.2%~9.0%。方法的检出限为0.3μg/kg。结论该方法灵敏、快捷、准确,适用于土壤中PCP的检测。
Objective The method of determination of pentachlorophenol was established in soil by solid-phase extraction-gas chromatography-mass spectrometry（ SPE-GC-MS）. Methods Pentachlorophenol（ PCP） in soil was extracted under acidic condition with ethyl acetate / n-hexane（ 1∶1,V / V）,and the extraction fluid was purified by SLC solid-phase extraction column,and then eluted with acetonetrile,and derived using acetic anhydride. The DB-5MS capillary column was adopted for separation and finally the samples were determined with GC-MS,and quantified with 2,4-dibromophenol as the internal standard. Results When the concentration of pentachlorophenol was in the linear range of 2. 0 μg / kg-40 μg / kg,the equation of linear regression was y = 0. 056 2x ＋ 0. 001 4 with the correlation coefficient of 0. 999 6. The standard concentration of pentachlorophenol was among 2. 5 μg / kg-20. 0 μg / kg,and the average recovery rate of the method was in the range of 85. 6%-97. 0%,with RSDs of 5. 2%-9. 0%. The limit of the method detection was 0. 3 μg / kg. Conclusion This method is sensitive,rapid and accurate,and can be applied to the detection of PCP in soil.
出处
《中国卫生检验杂志》
CAS
2016年第5期622-624,共3页
Chinese Journal of Health Laboratory Technology
基金
浙江省嘉善县县级科技计划和专项资金项目(2013A40)
关键词
五氯酚
土壤
气相色谱-质谱法
测定
Pentachlorophenol
Soil
Gas chromatography-mass spectrometry
Determination
