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以可溶解层状双氢氧化物空心球为吸附剂的注射器内分散固相萃取结合高效液相色谱法测定河水中的11种酚类物质

In-syringe dispersive solid-phase extraction using dissolvable layered double oxide hollow spheres as sorbent followed by high-performance liquid chromatography for determination of 11 phenols in river water.

作者信息

Tang Sheng, Lin Xuan Hao, Li Sam Fong Yau, Lee Hian Kee

机构信息

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.

出版信息

J Chromatogr A. 2014 Dec 19;1373:31-9. doi: 10.1016/j.chroma.2014.11.031. Epub 2014 Nov 21.

Abstract

Layered double oxide hollow spheres (LDO-HSs) were synthesized and employed as a dissolvable sorbent in dispersive solid-phase extraction (DSPE) to extract eleven United States Environmental Protection Agency's priority phenols from aqueous samples. With their higher specific surface area, LDO-HSs showed much higher extraction efficiency than normal layered double hydroxides and layered double oxides. The entire extraction process was accomplished in a syringe. After DSPE, the sorbent with the analytes was isolated conveniently by directly expelling the spent sample solution out of the syringe. The analyte-enriched sorbent was then subsequently dissolved by withdrawing an acidic solution into the syringe. The final extract was analyzed by high-performance liquid chromatography with ultraviolet detection. The results showed that this method provided low limits of detection for the phenols (0.005-0.153 μg/L), good linearity (r(2)≥ 0.9956) and relative standard deviations of ≤ 6.7%. The optimized method was applied to water samples from 3 rivers. This simple extraction procedure was demonstrated to be a fast, efficient and convenient DSPE approach.

摘要

合成了层状双金属氢氧化物空心球(LDO-HSs),并将其用作分散固相萃取(DSPE)中的可溶解吸附剂,用于从水样中萃取美国环境保护局规定的11种优先酚类物质。由于具有较高的比表面积,LDO-HSs的萃取效率比普通层状双金属氢氧化物和层状双金属氧化物高得多。整个萃取过程在注射器中完成。DSPE后,通过直接将用过的样品溶液从注射器中排出,可方便地分离出带有分析物的吸附剂。然后,通过向注射器中注入酸性溶液,使富集了分析物的吸附剂溶解。最终提取物采用高效液相色谱-紫外检测法进行分析。结果表明,该方法对酚类物质的检测限较低(0.005-0.153μg/L),线性良好(r(2)≥0.9956),相对标准偏差≤6.7%。该优化方法应用于3条河流的水样。这种简单的萃取程序被证明是一种快速、高效且便捷的DSPE方法。

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