Highly selective solid phase extraction and preconcentration of Azathioprine with nano-sized imprinted polymer based on multivariate optimization and its trace determination in biological and pharmaceutical samples

•The nanosized-imprinted polymer has been synthesized by precipitation polymerization technique.•A molecularly imprinted solid-phase extraction procedure was performed for determination of Azathioprine.•The Azathioprine-molecular imprinting polymer can be considered for quality control of pharmaceutical preparations.•In order to investigate the effect of variables, the Box-Behnken Design (BBD) under Response Surface Methodology (RSM) was employed.

In this research, for first time selective separation and determination of Azathioprine is demonstrated using molecularly imprinted polymer as the solid-phase extraction adsorbent, measured by spectrophotometry at λmax 286 nm. The selective molecularly imprinted polymer was produced using Azathioprine and methacrylic acid as a template molecule and monomer, respectively. A molecularly imprinted solid-phase extraction procedure was performed in column for the analyte from pharmaceutical and serum samples. The synthesized polymers were characterized by infrared spectroscopy (IR), field emission scanning electron microscopy (FESEM). In order to investigate the effect of independent variables on the extraction efficiency, the response surface methodology (RSM) based on Box-Behnken design (BBD) was employed. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions and the proposed method was applied to analysis of Azathioprine. The linear dynamic range and limits of detection were 2.5-0.01 and 0.008 mg L‐ 1 respectively. The recoveries for analyte were higher than 95% and relative standard deviation values were found to be in the range of 0.83-4.15%. This method was successfully applied for the determination of Azathioprine in biological and pharmaceutical samples.

Graphical abstractA new-nano sized imprinted polymer was synthesized and applied as sorbent in SPE in order to selective recognition, preconcentration, and determination of Azathioprine with the response surface methodology based on Box-Behnken design and was successfully investigated for the clean-up of human blood serum and pharmaceutical samples.Download high-res image (188KB)Download full-size image