摘要
建立了基于微波辅助-顶空液相微萃取在线联用、高效液相色谱法测定水样中邻硝基苯酚的分析方法。采用L16(45)正交实验设计对影响萃取的各种因素,如萃取有机溶剂、微波辐射功率、萃取时间、离子强度、样品液体积,进行了优化。优化后萃取条件为,以乙酸丁酯作为萃取溶剂,功率和时间分别为100W和12min条件下,离子强度为0的样品溶液体积为20mL。在优化萃取条件下,邻硝基苯酚的检出限LOD(S/N=3)为0.94μg/L,萃取富集倍数为30,实际水样的加标回收率为85.2%。理论分析和实验结果表明,微波辅助-顶空液相微萃取在线联用方法具有简便、快速、高效、节省溶剂、选择性好、应用范围广的特点。
The method for the determination of 2-Nitrophenol in environmental water samples had been developed using microwave-assisted-headspace-liquid-phase microextraction(MA-HS-LPME) coupled with high performance liquid chromatography(HPLC).The variable experimental conditions for the MA-HS-LPME extraction process,including extraction solvent,microwave irradiation power,extraction time,contents of inorganic salt and sample volume,were optimized by L16(45) orthogonal design.The optimized method was as following: butyl acetate as organic drop,20 mL aqueous sample without NaCl addition extracting for 12 min under microwave irradiation power 100 W.Under the optimized conditions,low detection limit(S/N=3) and the enrichment factor of the method for the target compound were 0.94μg/L and 30,respectively.The recoveries of target analyte spiked real water samples were 85.2%.The results indicated that the developed method is simple,rapid,efficient,solvent-saving,highly selective and widely applicable.
出处
《化学通报》
CAS
CSCD
北大核心
2011年第12期1140-1144,共5页
Chemistry
基金
重庆市教育委员会科学技术研究项目(KJ100102)
中央高校基本科研业务费项目(CDJXS10220004)资助
关键词
微波辅助萃取
顶空液相微萃取
高效液相色谱
邻硝基苯酚
Microwave-assisted extraction(MAE)
Headspace-liquid-phase microextraction(HS-LPME)
High performance liquid chromatography(HPLC)
2-Nitrophenol