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水中极性酚类的搅拌棒吸附萃取结合在聚乙烯吡咯烷酮 - 二乙烯基苯整体柱中进行高效液相色谱分离的方法开发与验证

Development and validation of stir bar sorptive extraction of polar phenols in water followed by HPLC separation in poly(vinylpyrrolididone-divinylbenzene) monolith.

作者信息

Huang Xiaojia, Qiu Ningning, Yuan Dongxing

机构信息

State Key Laboratory of Marine Environmental Science, Environmental Science Research Center, Xiamen University, Xiamen, China.

出版信息

J Sep Sci. 2009 May;32(9):1407-14. doi: 10.1002/jssc.200800708.

Abstract

An effective and simple method for polar phenols in water matrix was developed by using stir bar sorptive extraction (SBSE) based on a hydrophilic poly(vinylpyrrolididone-divinylbenzene) (VPDB) monolithic material and HPLC analysis. To achieve optimum extraction performance for phenols, several parameters, including extraction and desorption time, desorption solvent, pH value, and ionic strength of sample matrix, were investigated. Under the optimized experimental conditions, eight phenols were directly enriched from water samples and analyzed by HPLC-DAD. The detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.72-1.37 and 2.40-4.27 ng/mL from spiked water, respectively. Recoveries of eight phenolic compounds were found in the range of 55.2-95.9%. The calibration curves showed the linearity ranging from 5 to 150 ng/mL with linear regression coefficient R(2) values above 0.98. Method repeatability presented as intra- and interday precisions were also found with the RSDs less than 4.10 and 7.61%, respectively. The distribution coefficients between VPDB and water (K(VPDB/W)) for phenolic compounds were also calculated and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the target compounds in tap water, sea water and wastewater samples.

摘要

基于亲水性聚(乙烯基吡咯烷酮 - 二乙烯基苯)(VPDB)整体材料的搅拌棒吸附萃取(SBSE)和高效液相色谱分析,开发了一种用于水基质中极性酚类的有效且简单的方法。为实现酚类的最佳萃取性能,研究了几个参数,包括萃取和解吸时间、解吸溶剂、pH值以及样品基质的离子强度。在优化的实验条件下,从水样中直接富集8种酚类并用高效液相色谱 - 二极管阵列检测器(HPLC - DAD)进行分析。该方法对加标水样中目标化合物的检测限(S/N = 3)和定量限(S/N = 10)分别在0.72 - 1.37和2.40 - 4.27 ng/mL范围内。8种酚类化合物的回收率在55.2 - 95.9%范围内。校准曲线的线性范围为5至150 ng/mL,线性回归系数R²值高于0.98。方法的重复性以日内和日间精密度表示,相对标准偏差(RSD)分别小于4.10%和7.61%。还计算了酚类化合物在VPDB与水之间的分配系数(K(VPDB/W))并与K(O/W)进行比较。最后,该方法成功应用于自来水、海水和废水样品中目标化合物的测定。

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