Department of Environmental Science and Engineering, Sichuan University, Chengdu, China.
J Sep Sci. 2012 Oct;35(20):2796-804. doi: 10.1002/jssc.201200234. Epub 2012 Aug 15.
A simple, rapid, and efficient method, vortex-assisted extraction followed by dispersive liquid-liquid microextraction (DLLME) has been developed for the extraction of polycyclic aromatic hydrocarbons (PAHs) in sediment samples prior to analysis by high performance liquid chromatography fluorescence detection. Acetonitrile was used as collecting solvent for the extraction of PAHs from sediment by vortex-assisted extraction. In DLLME, PAHs were rapidly transferred from acetonitrile to dichloromethane. Under the optimum conditions, the method yields a linear calibration curve in the concentration range from 10 to 2100 ng g(-1) for fluorene, anthracene, chrysene, benzo[k]fluoranthene, and benzo[a]pyrene, and 20 to 2100 ng g(-1) for other target analytes. Coefficients of determinations ranged from 0.9986 to 0.9994. The limits of detection, based on signal-to-noise ratio of three, ranged from 2.3 to 6.8 ng g(-1) . Reproducibility and recoveries was assessed by extracting a series of six independent sediment samples, which were spiked with different concentration levels. Finally, the proposed method was successfully applied in analyses of real nature sediment samples. The proposed method extended and improved the application of DLLME to solid samples, which greatly shorten the extraction time and simplified the extraction process.
一种简单、快速、高效的方法,涡旋辅助萃取(Vortex-assisted extraction)后结合分散液液微萃取(Dispersive liquid-liquid microextraction,DLLME),已被开发用于分析前从沉积物样品中提取多环芳烃(Polycyclic aromatic hydrocarbons,PAHs)。乙腈被用于通过涡旋辅助萃取从沉积物中萃取 PAHs。在 DLLME 中,PAHs 迅速从乙腈转移到二氯甲烷中。在最佳条件下,该方法对芴、蒽、䓛、苯并[k]荧蒽和苯并[a]芘的浓度范围为 10 至 2100ng/g,其他目标分析物的浓度范围为 20 至 2100ng/g,均得到线性校准曲线。相关系数范围为 0.9986 至 0.9994。基于信噪比为 3 的检测限范围为 2.3 至 6.8ng/g。通过提取一系列 6 个独立的沉积物样品并对其进行不同浓度水平的加标,评估了重现性和回收率。最后,该方法成功应用于实际自然沉积物样品的分析。该方法扩展和改进了 DLLME 在固体样品中的应用,大大缩短了萃取时间并简化了萃取过程。