分散液相微萃取-气相色谱法测定水样中的多溴联苯醚
来源期刊：中南大学学报(自然科学版)2012年第10期
论文作者：王丹丹 黄卫红 黄婷婷 徐婉珍 杨岚钦 周威
文章页码：4159 - 4164
关键词：分散液相微萃取；气相色谱；多溴联苯醚；水样
Key words：dispersive liquid-liquid microextraction; gas chromatography-electron capture detection; polybrominated diphenyl ethers; water samples
摘 要：建立分散液相微萃取(DLLME)与气相色谱-电子捕获检测器(GC-ECD)联用技术快速测定水样中多溴联苯醚(PBDEs)的新方法。考察萃取剂和分散剂的种类、萃取剂用量、分散剂用量、萃取时间和离子强度等因素对目标物萃取效率和富集因子的影响。用单因素实验进行优化，得到最佳萃取条件为：1.0 mL丙酮作分散剂，30 μL四氯乙烷作萃取剂，萃取时间为5 min，不加盐(NaCl)。在最佳萃取条件下，该方法溶液质量浓度的线性范围为0.1~50 μg/L(线性相关系数r2=0.998 3)，相对标准偏差为8.6%，检出限为15.2 ng/L(信噪比为3)。将该方法用于生活污水和海水的分析检测，均检出4,4’-二溴联苯醚(BDE-15)，平均加标回收率分别为93.5%和92.5%，相对标准偏差分别为9.3%和7.9%。该方法可对水样中痕量多溴联苯醚进行快速准确检测，结果令人满意。
Abstract: A novel method based on dispersive liquid-liquid microextraction (DLLME) and gas chromatography- electron capture detection (GC-ECD) was developed for the determination of polybrominated diphenyl ethers (PBDEs) in water samples. The effective parameters, such as the type and volume of extraction solvents and disperser solvents, extraction time and ionic strength were investigated. The optimal conditions are as follows: 1.0 mL acetone as disperser solvent, 30 μL C2H2Cl4 as extraction solvent, 5 min extraction time and no salt. Under the optimum extraction condition, the method yields a good linear relationship in the mass concentration range of 0.1-50 μg/L with the correlation coefficient of 0.998 3. The relative standard deviations (RSDs) is 8.6% and the limit of detection (LODs), based on signal-to-noise (S/N) of 3, is 15.2 ng/L. The proposed method is applied in the determination of domestic sewage and seawater, in both of which BDE-15 is found. The average recoveries of BDE-15 from the samples are 93.5% and 92.5% respectively with RSDs 9.3% and 7.9%. The developed method can be used for the determination of trace level PBDEs in water samples.
王丹丹，黄卫红，黄婷婷，徐婉珍，杨岚钦，周威
(江苏大学 环境学院，江苏 镇江，212013)
摘 要：建立分散液相微萃取(DLLME)与气相色谱-电子捕获检测器(GC-ECD)联用技术快速测定水样中多溴联苯醚(PBDEs)的新方法。考察萃取剂和分散剂的种类、萃取剂用量、分散剂用量、萃取时间和离子强度等因素对目标物萃取效率和富集因子的影响。用单因素实验进行优化，得到最佳萃取条件为：1.0 mL丙酮作分散剂，30 μL四氯乙烷作萃取剂，萃取时间为5 min，不加盐(NaCl)。在最佳萃取条件下，该方法溶液质量浓度的线性范围为0.1~50 μg/L(线性相关系数r2=0.998 3)，相对标准偏差为8.6%，检出限为15.2 ng/L(信噪比为3)。将该方法用于生活污水和海水的分析检测，均检出4,4’-二溴联苯醚(BDE-15)，平均加标回收率分别为93.5%和92.5%，相对标准偏差分别为9.3%和7.9%。该方法可对水样中痕量多溴联苯醚进行快速准确检测，结果令人满意。
关键词：分散液相微萃取；气相色谱；多溴联苯醚；水样
WANG Dan-dan, HUANG Wei-hong, HUANG Ting-ting, XU Wan-zhen, YANG Lan-qin, ZHOU Wei
(School of Environment, Jiangsu University, Zhenjiang 212013, China)
Abstract:A novel method based on dispersive liquid-liquid microextraction (DLLME) and gas chromatography- electron capture detection (GC-ECD) was developed for the determination of polybrominated diphenyl ethers (PBDEs) in water samples. The effective parameters, such as the type and volume of extraction solvents and disperser solvents, extraction time and ionic strength were investigated. The optimal conditions are as follows: 1.0 mL acetone as disperser solvent, 30 μL C2H2Cl4 as extraction solvent, 5 min extraction time and no salt. Under the optimum extraction condition, the method yields a good linear relationship in the mass concentration range of 0.1-50 μg/L with the correlation coefficient of 0.998 3. The relative standard deviations (RSDs) is 8.6% and the limit of detection (LODs), based on signal-to-noise (S/N) of 3, is 15.2 ng/L. The proposed method is applied in the determination of domestic sewage and seawater, in both of which BDE-15 is found. The average recoveries of BDE-15 from the samples are 93.5% and 92.5% respectively with RSDs 9.3% and 7.9%. The developed method can be used for the determination of trace level PBDEs in water samples.
Key words:dispersive liquid-liquid microextraction; gas chromatography-electron capture detection; polybrominated diphenyl ethers; water samples
