Article ID Journal Published Year Pages File Type
1213225 Journal of Chromatography B 2012 6 Pages PDF
Abstract

A porous poly(N-isopropylacrylamide-co-ethyleneglycol dimethacrylate) [poly(NIPAAm-co-EDMA)] monolithic column was prepared by in situ free-radical polymerization. The morphology of monolithic column and pressure drop across the columns were characterized. The results showed excellent permeability and high selectivity. Nifedipine, nitrendipine and nisoldipine were simultaneously selected to validate the extraction efficiency of the prepared monolith both in plasma and urine. The extracted nifedipine, nitrendipine and nisoldipine from plasma and urine samples have been on-line tested quantitatively by using the prepared monolith connected with RP-C18 column. The total analytical run time was 38 min. For all analytes, linear calibration curves were obtained over a range of 2–500 ng/mL with coefficient of correlation > 0.997. Precision for inter- and intra-day assay showed acceptable results for quantitative assay with relative standard deviation (RSD) less than 12%. The accuracy and recovery was found to be in the range of 89–109% and 88–106%. The results indicated that the prepared monolith was feasible to be used as an on-line SPE sorbent material and the method was especially appropriate for multi-analytes monitoring in plasma and urine samples. Finally, the proposed method was successfully applied to simultaneously screen nifedipine, nitrendipine and nisoldipine in plasma.

► A porous poly(N-isopropylacrylamide-co-ethyleneglycol dimethacrylate) [poly(NIPAAm-co-EDMA)] monolithic column was prepared by in situ free-radical polymerization. ► The prepared poly(NIPAAm-co-EDMA) monolithic column showed excellent permeability and high selectivity, which was suitable for SPE pre-column. ► The prepared poly(NIPAAm-co-EDMA) monolithic column was used as SPE sorbent to simultaneously clean up of protein and enrich of nifedipine, nitrendipine and nisoldipine in plasma and urine. ► The sample pretreatment step was embedded into the LC chromatographic system and manual intervention was minimized. ► The established method was also applied in clinical plasma studies.

Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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