摘要
建立了超声波提取-气相色谱法同时测定土壤中21种酚类化合物的分析方法.用二氯甲烷和正己烷混合溶剂提取土壤中的酚类化合物,提取液经碱性水溶液分配净化,去除非酸性有机杂质,再酸化萃取酚类化合物,浓缩后采用气相色谱-氢火焰离子化检测器进行检测,外标法定量.以10g土壤样品计,酚类化合物的检出限为0.01~0.06 mg/kg.实际样品添加回收试验的回收率为62.9%~111.4%,相对标准偏差为4.3% ~ 24.0%(n=6),准确度和精密度均较好.结果表明:该法操作方便,净化效果好,可用于土壤中多种酚类化合物的测定.
An effective method was developed to determine phenolic compounds in soil by ultrasonic extraction-gas chromatography (GC).The soil sample was extracted with methylene dichloride-hexane (2∶ 1,v/v) for 3 min with the extraction temperature lower than 50 ℃ for 3 times.The extract was purified by alkaline aqueous solution (pH 〉 12),and the phenolic compounds were dissolved in aqueous solution.After the organic solution was discarded,the aqueous solution was adjusted to pH 〈 3 and subsequently extracted with methylene dichloride-ethyl acetate (4∶ 1,v/v) twice.The analytes were determined by GC-FID and quantified by external standard method.The limits of quantification for all tested phenolic compounds were 0.01-0.06 mg/kg in about 10 g soil samples.The recoveries were between 62.9% and 111.4% with the relative standard deviations (RSDs) in the range of 4.3%-24.0% (n =6).The results showed that this method is sensitive,accurate,and suitable for the determination of the 21 phenolic compounds in soil.
出处
《色谱》
CAS
CSCD
北大核心
2013年第11期1081-1086,共6页
Chinese Journal of Chromatography
基金
国家环境保护标准制修订项目(2009-1045)
南京市建设委员会科技项目(200717J)
关键词
超声波提取
气相色谱法
酚类化合物
土壤
ultrasonic extraction
gas chromatography (GC)
phenolic compounds
soil