Temperature responsive chromatography for therapeutic drug monitoring with an aqueous mobile phase

Therapeutic drug monitoring is a key technology for effective pharmacological treatment. In the present study, a temperature-responsive chromatography column was developed for safe and simple therapeutic drug monitoring without the use of organic solvents. Poly(N-isopropylacrylamide) (PNIPAAm) hydrogel-modified silica beads were prepared via a condensation reaction and radical polymerization. The temperature-dependent elution behavior of the drugs was observed using a PNIPAAm-modified silica-bead packed column and an all-aqueous mobile phase. Sharp peaks with reproducible retention times were observed at temperatures of 30 °C or 40 °C because the PNIPAAm hydrogel on the silica beads shrinks at these temperatures, limiting drug diffusion into the PNIPAAm hydrogel layer. The elution behavior of the sample from the prepared column was examined using a mixture of serum and model drugs. The serum and drugs were separated on the column at 30 °C or 40 °C, and the concentration of the eluted drug was obtained using the calibration curve. The results show that the prepared chromatography column would be useful for therapeutic drug monitoring because the drug concentration in serum can be measured without using organic solvents in the mobile phase and without any need for sample preparation.

Effect of pore diameter on the elution behavior of analytes from thermoresponsive polymer grafted beads packed columns

Temperature-responsive chromatography using thermoresponsive polymers is innovative and can control analyte retention via column temperature. Analyte elution behavior in this type of chromatography depends on the modified thermoresponsive polymer and the structure of the base materials. In the present study, we examine the effect of the pore diameter of silica beads on analyte elution behavior in temperature-responsive chromatography. Poly(N-isopropylacrylamide-co-n-butyl methacrylate) hydrogel was applied to beads of various pore sizes: 7, 12, and 30 nm. Almost the same amount of copolymer hydrogel was applied to all beads, indicating that the efficiency of copolymer modification was independent of pore size. Analyte retention on prepared beads in a packed column was observed using steroids, benzodiazepines, and barbiturates as analytes. Analyte retention times increased with temperature on packed columns of 12- and 30-nm beads, whereas the column packed with 7-nm beads exhibited decreased retention times with increasing temperature. The difference in analyte elution behavior among the various pore sizes was attributed to analyte diffusion into the bead pores. These results demonstrate that bead pore diameter determines temperature-dependent elution behavior.

Relationship between the formation of flow paths and elution behavior with water flow through the soil column

<p>The transport phenomenon of pollutants in soil is complicated because of the formation of the flow path in soil. In this study, the relationship between the flow path in the soil and the elution behavior of various components was evaluated by the column tests with different filling methods to change the flow path in the column. The flow path in the column was visualized by using potassium iodide aqueous solution and X-ray CT. Our result shows that the elution behavior of the easily eluted components was not significantly affected by the flow path in the column. In addition, the cation more eluted when the flow path spread throughout the column than when the flow path was intensive. This suggests that eluted components may be affected by anions in soil. From these results, it was found that the elution behavior of components is influenced by the flow path in the column and some were not, and when it was influenced, the degree of influence is different depending on the components.</p>