超声提取/高效液相色谱法测定土壤中的4-壬基酚

在考察不同提取方法和有机溶剂提取效率的基础上，建立了土壤样品中内分泌干扰物4-壬基酚（4-NP）的超声提取/高效液相色谱(紫外检测器)分析方法。结果显示，以二氯甲烷作提取溶剂时超声提取对土壤中4-NP的提取效率高于索氏提取法；不同有机溶剂的超声提取效率依次为二氯甲烷-甲醇(9∶1)＞二氯甲烷＞甲醇≈丙酮。样品采用二氯甲烷-甲醇(9∶1)超声提取，经硅胶柱净化、高效液相色谱检测，土壤在4-NP的高、中、低3个加标水平下的平均回收率为91%~94%，相对标准偏差为4.3%~7.2%，方法的检出限为2.0 μg/kg。采用该方法对广东省部分土壤中的4.NP进行检测，得到其含量为5.3~16 μg/kg(干重)，低于河北省污水灌溉土壤中的含量。该方法简便快捷、灵敏、重现性好，适用于土壤样品中4-NP的分析。

Determination of 4-Nonylphenol in Soil by Ultrasonic-assisted Extraction and High Performance Liquid Chromatography

Based on the comparison of extraction efficiencies of two extraction methods and different organic solvents,an ultrasonic-assisted extraction procedure coupled with high performance liquid chromatography(HPLC) with UV detector was developed for the determination of 4-nonylphenol(4-NP) in soil.The results showed that the extraction efficiency of 4-NP in soil by ultrasonic-assisted extraction with dichloromethane was higher than that by the Soxhlet-extraction method.The results of ultrasonic-assisted extraction with different organic solvents demonstrated that the extraction efficiencies decreased in an order of dichloromethane-methanol(9 ∶ 1)>dichloromethane>methanol≈acetone.The recoveries of 4-NP in soil at three spiked levels of 10,20,40 mg/kg ranged from 91% to 94% with relative standard deviations(RSDs) of 4.3%-7.2%,and the detection limit of method for 4-NP was 2.0 μg/kg.The method was applied in the determination of 4-NP in soil samples collected from Guangdong Province,and the results showed that the concentrations of 4-NP varied from 5.3 μg/kg to 16 μg/kg by dry weight,which were lower than those obtained from the wastewater irrigated soil of Hebei Province.This method is rapid,sensitive,reproducible and suitable for the determination of 4-NP in soil.