超声提取/高效液相色谱法测定土壤中的4-壬基酚

摘要

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 n-g/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.%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2.0μg/k g.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.