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| 气相色谱-电子捕获检测法测定海水中十氯酮残留 | |
| 引用本文： | 王艳洁,那广水,王震,姚子伟. 气相色谱-电子捕获检测法测定海水中十氯酮残留[J]. 色谱, 2012, 30(8): 847-850. DOI: 10.3724/SP.J.1123.2012.04013 |
| 作者姓名： | 王艳洁 那广水 王震 姚子伟 |
| 作者单位： | (国家海洋局近岸海域生态环境重点实验室 国家海洋环境监测中心, 辽宁 大连 116023 |
| 基金项目： | 海洋公益性行业科研专项经费项目(201105013);国家海洋局近岸海域生态环境重点实验室开放基金项目(201110) |
| 摘 要： | 通过考察提取溶剂、毛细管柱、净化条件及共溶出干扰物等因素对十氯酮测定的影响,建立了二氯甲烷液-液富集萃取、硫酸净化分离、气相色谱法(GC)-电子捕获检测器(ECD)测定海水介质中有机氯农药类持久性有机污染物十氯酮残留分析方法。1 L海水经50 mL二氯甲烷萃取富集,浓缩后采用硫酸净化,以1%(体积分数)甲醇/正己烷混合溶液转移定容后,采用DB-5非极性毛细管柱进行GC分离,电子捕获检测器可测定其中十氯酮的含量;该方法采用外标法定量,在5～100 μg/L范围内呈线性,线性相关系数为0.9989。低、中、高3个浓度水平的平均加标回收率为81%～108%,相对标准偏差为1.2%～5.1%(n=6)。方法的检出限为0.6 ng/L。结果表明,该方法灵敏度高,线性关系好,可以满足简便、快速、准确测定海水中十氯酮的要求。 |
| 关 键 词： | 电子捕获检测器 海水 气相色谱法 十氯酮 |
| 收稿时间： | 2012-04-09 |
Determination of kepone residue in seawater by gas chromatography coupled with electron capture detector |
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| WANG Yanjie,NA Guangshui,WANG Zhen,YAO Ziwei. Determination of kepone residue in seawater by gas chromatography coupled with electron capture detector[J]. Chinese journal of chromatography, 2012, 30(8): 847-850. DOI: 10.3724/SP.J.1123.2012.04013 | |
| Authors: | WANG Yanjie NA Guangshui WANG Zhen YAO Ziwei |
| Affiliation: | Key Laboratory for Ecological Environment in Coastal Areas of State Oceanic Administration, National Marine Environmental Monitoring Center, Dalian 116023, China |
| Abstract: | The effects of extraction solvent,capillary column,cleanup method,co-eluted analytes and other influencing factors on the detection of kepone in seawater were investigated.The analytical method of gas chromatography(GC) coupled with electron capture detector(ECD) was established to determine kepone in seawater.In the method,liquid-liquid extraction and sulfuric acid cleanup were used in the sample pre-processing.Chromatographic analysis was performed on a DB-5 capillary column with external standard method.The kepone was extracted from a 1 L seawater sample by 50 mL dichloromethane.Sulfuric acid was used to remove the interference materials co-extracted from the sample.After cleanup,the extract was dissolved in 1%(v/v) methanol/hexane solvent and analyzed by GC-ECD.In the linear range from 5 μg/L to 100 μg/L of kepone,the correlation coefficient was 0.9989.The average spiked recoveries were 81%-108% with the relative standard deviations(RSDs) of 1.2%-5.1%(n=6).The detection limit was 0.6 ng/L.This method shows good extraction efficiency,high sensitivity and good reproducibility,and is suitable for the determination of kepone in seawater. |
| Keywords: | gas chromatography(GC) electron capture detector(ECD) kepone seawater |
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