Su Rihui, Ruan Guihua, Chen Zhengyi, Du Fuyou, Li Jianping
Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi, China.
J Sep Sci. 2015 Dec;38(24):4262-8. doi: 10.1002/jssc.201500580. Epub 2015 Nov 24.
A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%.
一种新型的固相萃取柱由接枝巯基二氧化硅聚合高内相乳液颗粒制备而成,用于痕量铅的预富集。首先,通过高内相乳液聚合合成巯基二氧化硅聚合高内相乳液颗粒,并小心地组装在聚乙烯注射器柱中。分别优化了包括吸附pH值、吸附和解吸溶剂、吸附和解吸过程流速等各种参数的影响,还研究了合适的上样体积、吸附容量和固相萃取柱的可重复使用性。在最佳条件下,Pb(2+)可在较宽的pH范围(2.0 - 5.0)内进行定量预富集。在存在诸如Na(+)、K(+)、Ca(2+)、Zn(2+)、Mg(2+)、Cu(2+)与Fe(2+)、Cd(2+)、Cl(-)和NO3 (-)等外来离子的情况下,Pb(2+)能够成功回收。所制备的固相萃取柱具有高稳定性和良好的耐用性,可进行超过100次重复萃取而性能无明显变化。通过对大米样品中Pb(2+)的萃取进一步验证了所开发方法的可行性。在40.0、200和800 μg/kg三个加标水平下,大米样品中Pb(2+)的平均回收率在87.3%至105.2%之间。