摘要
建立了测定环境水样中7种萘二酚的离子液体分散液液微萃取/高效液相色谱(IL-DLLME-HPLC)分析方法。以1-丁基-3-甲基咪唑六氟磷酸盐([C4MIM][PF6])为萃取剂,水样体积为8.0 m L,研究了萃取剂用量、水相p H值、萃取时间及盐添加量对7种萘二酚萃取效率的影响。获得最佳萃取条件为:[C4MIM][PF6]体积为150μL,水相p H值为5.0~7.0,涡旋萃取时间为3 min,氯化钠添加量为0.20 g/m L。在优化条件下,7种萘二酚在一定质量浓度范围内线性关系良好,相关系数均不小于0.997 7;方法富集倍数为57倍,方法检出限(S/N=3)为0.3~1.0μg/L;阴性环境水样中3个加标水平的平均回收率为83.5%~103%,相对标准偏差(n=6)为1.1%~3.8%。该方法快速简单、准确灵敏、环保,适用于环境水样中痕量萘二酚的富集检测。
A sensitive method based on ionic liquid dispersive liquid -liquid microextraction (IL - DLLME) and high performance liquid chromatography with diode array detector( HPLC -PDA) was developed for the preconcentration and determination of seven naphthalenediols in environmental water samples. The ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ( [ C4 MIM ] [ PF6 ] ) was used as extraction agent, and 8.0 mL of aqueous phase was selected. Some important factors affect- ing the extraction efficiency such as amount of [ C4MIM] [ PF6 ], pH value of aqueous phase, extrac- tion time and salt concentration were optimized. The optimized conditions were as follows: 150μL [ C4 MIM ] [ PF6 ], pH value of aqueous solution : 5.0 - 7.0, vortex extraction time : 3 min, sodium chloride : 0. 20 g/mL. Under the optimized conditions, the calibration curves of 7 naphthalenediols were linear in the certain concentration range with correlation coefficients not less than O. 997 7. The enrichment factor of this method was 57, and the detection limits of this method ( S/N = 3 ) were be- tween 0.3 μg/L and 1.0 μg/L. The average recoveries of naphthalenediols at three spiked levels in negative environmental water sample ranged from 83.5% to 103% with relative standard deviations (RSD, n =6) of 1.1% -3. 8%. The developed method is rapid, sensitive and environment-friendly, and is suitable for the detection of trace naphthalenediols in environmental water samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第7期844-848,共5页
Journal of Instrumental Analysis
关键词
离子液体分散液液微萃取
高效液相色谱法
萘二酚
环境水样
ionic liquid dispersive liquid -liquid microextraction( IL- DLLME)
high performanceliquid chromatography(HPLC)
naphthalenediol
environmental water sample
作者简介
通讯作者:何东,讲师,研究方向:色谱质谱检测方法,Tel:0753-2523203,E-mail:gdone@tom.com