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基于顺序注射固-液萃取结合高效液相色谱法测定苯巴比妥和苯妥英的改进型分散液相微萃取。

Modified dispersive liquid-phase microextraction based on sequential injection solidified floating organic drop combined with HPLC for the determination of phenobarbital and phenytoin.

机构信息

Department of Chemistry, Faculty of Science, Yazd University, Yazd, Iran.

Department of Chemistry, Behbahan Khatam Alanbia University of Technology, Behbahan, Iran.

出版信息

J Sep Sci. 2018 Jan;41(2):509-517. doi: 10.1002/jssc.201701111. Epub 2017 Dec 11.

Abstract

A modified dispersive liquid phase microextraction based on sequential injection solidified floating organic drop was developed for simultaneous separation/preconcentration of trace amounts of phenobarbital and phenytoin. The important factors affecting on the extraction recovery including pH, the volume of extraction solvent, ionic strength, and the number of injections were investigated and optimized by Box-Behnken design and desirability function. Under the optimum experimental conditions, the calibration graph was linear in the concentration range of 1.0-300.0 μg/L (r = 0.997) for phenobarbital and 2.0-400.0 μg/L (r = 0.996) for phenytoin. The limit of detection and limit of quantification were 0.35 and 1.2 μg/L for phenobarbital and 0.65 and 2.2 μg/L for phenytoin, respectively. The relative standard deviation for six replicate determinations at 10 μg/L was 3.3 and 4.1% for phenobarbital and phenytoin, respectively. The developed method was successfully applied to the determination of phenobarbital and phenytoin in urine and plasma samples.

摘要

基于顺序注射固-浮有机液滴分散液相微萃取法,建立了一种同时分离/预浓缩痕量苯巴比妥和苯妥英的方法。通过 Box-Behnken 设计和理想性函数,考察并优化了影响萃取回收率的重要因素,包括 pH 值、萃取溶剂体积、离子强度和进样次数。在最佳实验条件下,苯巴比妥在 1.0-300.0μg/L 浓度范围内呈线性(r = 0.997),苯妥英在 2.0-400.0μg/L 浓度范围内呈线性(r = 0.996)。苯巴比妥的检出限和定量限分别为 0.35 和 1.2μg/L,苯妥英的检出限和定量限分别为 0.65 和 2.2μg/L。在 10μg/L 时,苯巴比妥和苯妥英的 6 次重复测定的相对标准偏差分别为 3.3%和 4.1%。该方法成功应用于尿液和血浆样品中苯巴比妥和苯妥英的测定。

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