涡旋辅助-液液萃取-气相色谱法测定土壤中水和甲醇可提态五氯酚  

Analyses of Water and Methanol Extractable Pentachlorophenol in Soils Using Vortex-assisted Liquid-liquid Extraction and Gas Chromatography

作　　者：于雄胜[1] 柳勇[1,2] 楼骏[1] 冯小莉[1] 汪海珍[1] 徐建明[1] 

机构地区：[1]浙江大学土水资源与环境研究所浙江省亚热带土壤与植物营养重点开放实验室,杭州310058 [2]广东省生态环境与土壤研究所广东省农业环境综合治理重点实验室,广州510650

出　　处：《分析化学》2015年第9期1389-1394,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.41171252;41090284;40701075)资助~~

摘　　要：建立了涡旋辅助-液液萃取-气相色谱测定土壤中水和甲醇可提态五氯酚（Pentachlorophenol,PCP）的方法。对涡旋转速、液液体积比等参数进行了优化,即涡旋转速为2000 r/min时PCP回收率最高,可达97.4%,重复性较好,相对标准偏差（RSD）为0.5%;衍生化溶液与正己烷的体积比为10∶4时PCP回收率为103%,RSD为0.7%。PCP提取测定的标准曲线线性范围为1.25~4000μg/L（R2=0.9999）,方法检出限在0.02μg/L以下,测量范围较宽,适合于痕量及微量PCP的分析。与传统液液萃取和固相萃取相比,本方法采用涡旋辅助萃取后有机溶剂消耗量最低、操作步骤最少,且测定的PCP回收率最高,可达96.8%。4种不同类型土壤经水提取一次和甲醇提取3次,在1和10 mg/kg PCP污染条件下,总回收率分别为89.5%~98.9%和88.7%~98.4%,说明本方法满足了不同类型土壤中水和甲醇可提态PCP在不同浓度范围内的提取测定要求。An analytical procedure for the determination of water- and methanol-extractable pentachlorophenol （PCP） in soils using vortex assisted liquid-liquid extraction （VALLE） and gas chromatography （GC） was developed. Significant extraction parameters, such as liquid-liquid ratio and vortex speed were optimized. The recovery of PCP was the highest （97. 4% ） at the vortex rotation speed of 2000 r/min, with good reproducbility and a small relative sdandard deviation （ RSD, 0.5% ）, with regard to the volume ratio of derivatization solution to n-hexane, the recovery of PCP was 103% with an RSD of 0.7% at 10： 4. The linearity of the calibration ranged from 1.25 μg/L to 4000 μg/L, with a correlation coefficient （ R2 ） of 0. 9999. The detection limit of the PCP in water was below 0.2 μg/L. Compared with traditional liquid-liquid extraction （LLE） and solid phase extraction （SPE） , the VALLE method was more simple and more economic in terms of chemical consumption, also with a recovery of 96.8% and a RSD of 3.7%. Four different soils were used to check the reliability of this method. The soils were respectively extracted with water once and methanol three times. The total recoveries were 89.5% -98.9% and 88.7% -98.4% at the PCP spiking level of 1 and 10 mg/kg, respectively. It is concluded that the VALLE method satisfied the extraction and determination of water and methanol extractable PCP in soils with varying PCP polluting rates.

关 键 词：五氯酚 涡旋辅助 液液萃取 水提态 甲醇可提态 土壤 

分 类 号：S151.9[农业科学—土壤学]