Novel core–shell SiO2@dSiO2@NH2-MIL-53(Al) packed into solid phase extraction column for enrichment of non-steroidal anti-inflammatory drugs prior to UPLC-MS/MS

Abstract

NH2-MIL-53(Al) was in situ synthesized on the SiO2@dSiO2 with a simple solvothermal method. The prepared composite was packed into column solid phase extraction as adsorbent. After introduction of SiO2@dSiO2 as the support, the drawbacks of adsorbent loss and high backpressure were overcome. Using ultra-high performance liquid chromatography-mass spectrometry, the proposed method was employed to analyze trace non-steroidal anti-inflammatory drugs (NSAIDs) in water samples. Extraction parameters, including type of adsorbent, pH of sample solution, flow rate, sample volume, type and volume of elution solvent, were optimized. Then commendable sensitivity was obtained with limits of detection from 0.5 to 4.0 pg·mL−1, and limits of quantification from 1.5 to 13.3 pg·mL−1. Moreover, the correlation coefficient (r) of linearity was 0.9916–0.9974. Satisfactorily, the recoveries of the target compounds were between 75.3 % and 109.3 %, and the relative standard deviation was less than 7.8 %. Furthermore, naproxen was chosen as a nominee to evaluate adsorption behavior of SiO2@dSiO2@NH2-MIL-53(Al). Molecular docking simulation calculations were conducted to explore adsorption mechanism between NH2-MIL-53(Al) and five NSAIDs.