Department of Chemistry, Faculty of Arts and Sciences, Zonguldak Karaelmas University, Zonguldak, Turkey.
J Sep Sci. 2012 Oct;35(19):2645-52. doi: 10.1002/jssc.201200317. Epub 2012 Aug 9.
A simple technique for the collection of an extraction solvent lighter than water after dispersive liquid-liquid microextraction combined with high-performance liquid chromatography with ultraviolet detection was developed for the determination of four paraben preservatives in aqueous samples. After the extraction procedure, low-density organic solvent together with some little aqueous phase was separated by using a disposable glass Pasteur pipette. Next, the flow of the aqueous phase was stopped by successive dipping the capillary tip of the pipette into anhydrous Na(2)SO(4). The upper organic layer was then removed simply with a microsyringe and injected into the high-performance liquid chromatography system. Experimental parameters that affect the extraction efficiency were investigated and optimized. Under optimal extraction conditions, the extraction recoveries ranged from 25 to 86%. Good linearity with coefficients with the square of correlation coefficients ranging from 0.9984 to 0.9998 was observed in the concentration range of 0.001-0.5 μg/mL. The relative standard deviations ranged from 4.1 to 9.3% (n = 5) for all compounds. The limits of detection ranged from 0.021 to 0.046 ng/mL. The method was successfully applied for the determination of parabens in tap water and fruit juice samples and good recoveries (61-108%) were achieved for spiked samples.
建立了一种在分散液液微萃取后,用比水轻的萃取溶剂收集的简单技术,并结合高效液相色谱-紫外检测法,用于测定水样中四种防腐剂的含量。萃取后,用一次性玻璃巴斯德吸管将低密度有机溶剂和一些少量水相分离。然后,通过连续将吸管的尖端浸入无水 Na(2)SO(4)来停止水相的流动。最后,只需用微量注射器将上层有机层取出并注入高效液相色谱系统。研究并优化了影响萃取效率的实验参数。在最佳萃取条件下,萃取回收率在 25%至 86%之间。在 0.001-0.5μg/mL 的浓度范围内,各化合物的线性关系良好,相关系数的平方均在 0.9984 至 0.9998 之间。相对标准偏差在 4.1%至 9.3%之间(n=5)。检出限在 0.021 至 0.046ng/mL 之间。该方法成功地应用于自来水中和果汁样品中防腐剂的测定,加标样品的回收率为 61%-108%。