Vidal Lorena, Psillakis Elefteria, Domini Claudia E, Grané Nuria, Marken Frank, Canals Antonio
Departamento de Química Analítica, Nutrición y Bromatología, Universidad de Alicante, P.O. Box 99, E-03080 Alicante, Spain.
Anal Chim Acta. 2007 Feb 12;584(1):189-95. doi: 10.1016/j.aca.2006.10.053. Epub 2006 Nov 7.
A headspace single-drop microextraction (HS-SDME) procedure using room temperature ionic liquid and coupled to high-performance liquid chromatography capable of quantifying trace amounts of chlorobenzenes in environmental water samples is proposed. A Plackett-Burman design for screening was carried out in order to determine the significant experimental conditions affecting the HS-SDME process (namely drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time and temperature), and then a central composite design was used to optimize the significant conditions. The optimum experimental conditions found from this statistical evaluation were: a 5 microL microdrop of 1-butyl-3-methylimidazolium hexafluorophosphate, exposed for 37 min to the headspace of a 10 mL aqueous sample placed in a 15 mL vial, stirred at 1580 rpm at room temperature and containing 30% (w/v) NaCl. The calculated calibration curves gave a high level of linearity for all target analytes with correlation coefficients ranging between 0.9981 and 0.9997. The repeatability of the proposed method, expressed as relative standard deviation, varied between 1.6 and 5.1% (n=5). The limits of detection ranged between 0.102 and 0.203 microg L(-1). Matrix effects upon extraction were evaluated by analysing spiked tap and river water as well as effluent water samples originating from a municipal wastewater treatment plant.
提出了一种采用室温离子液体的顶空单滴微萃取(HS-SDME)方法,并将其与高效液相色谱联用,用于定量分析环境水样中痕量氯苯。为了确定影响HS-SDME过程的重要实验条件(即液滴体积、水样体积、搅拌速度、离子强度、萃取时间和温度),进行了Plackett-Burman筛选设计,然后使用中心复合设计对重要条件进行优化。通过该统计评估找到的最佳实验条件为:5 μL 1-丁基-3-甲基咪唑六氟磷酸盐微滴,暴露于置于15 mL小瓶中的10 mL水样的顶空中37分钟,在室温下以1580 rpm搅拌,且含有30%(w/v)NaCl。计算得到的校准曲线对所有目标分析物都具有高度线性,相关系数在0.9981至0.9997之间。该方法的重复性以相对标准偏差表示,在1.6%至5.1%之间(n = 5)。检测限在0.102至0.203 μg L⁻¹之间。通过分析加标自来水、河水以及来自城市污水处理厂的出水水样,评估了萃取过程中的基质效应。