MCM-41 solid phase membrane tip extraction combined with liquid chromatography for the determination of non-steroidal anti-inflammatory drugs in human urine

• MCM-41 was successfully used as an adsorbent in solid phase membrane tip extraction (SPMTE).
• Seven parameters in SPMTE were optimized for extracting non-steroidal anti-inflammatory (NSAIDs) in human urine.
• Good recovery and satisfactory RSDs were achieved.
• The proposed methods were comparable with commercial-C18-SPE method for most of the NSAIDs.

Mesoporous silica material, MCM-41, was utilized for the first time as an adsorbent in solid phase membrane tip extraction (SPMTE) of non-steroidal anti-inflammatory drugs (NSAIDs) in urine prior to high performance liquid chromatography-ultraviolet (HPLC-UV) analysis. The prepared MCM-41 material was enclosed in a polypropylene membrane tip and used as an adsorbent in SPMTE. Four NSAIDs namely ketoprofen, diclofenac, mefenamic acid and naproxen were selected as model analytes. Several important parameters, such as conditioning solvent, sample pH, salting-out effect, sample volume, extraction time, desorption solvent and desorption time were optimized. Under the optimum extraction conditions, the MCM-41-SPMTE method showed good linearity in the range of 0.01–10 μg/mL with excellent correlation coefficients (r = 0.9977–0.9995), acceptable RSDs (0.4–9.4%, n = 3), good limits of detection (5.7–10.6 μg/L) and relative recoveries (81.4–108.1%). The developed method showed a good tolerance to biological sample matrices.