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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 To establish a SPE-GC-MS method for the determination of pentachlorophenol (PCP) in agricultural soils. Methods PCP in soil was extracted under acidic conditions with ethyl acetate-n-hexane (1: 1, V / V). The extract was purified by SLC SPE cartridge, eluted with acetonitrile and derivatized with acetic anhydride using DB- Capillary column separation, determination by GC-MS, 2,4-dibromophenol as internal standard. Results When the concentration of PCP was 2.0μg / kg ~ 40μg / kg, the linear relationship was good. The regression equation was y = 0.056x2 + 0.001 4 and the correlation coefficient was 0.999 6. The average recoveries ranged from 85.6% to 97.0% and the relative standard deviations (RSDs) ranged from 5.2% to 9.0% at spiked levels of 2.5 μg / kg to 20.0 μg / kg in soil. The detection limit of the method was 0.3 μg / kg. Conclusion The method is sensitive, fast and accurate and suitable for the detection of PCP in soil.