Comparison of the applicability of electromembrane extraction and liquid-phase microextraction for extraction of non-polar basic drugs from different biological samples: Using clozapine as the model analyte.

Understanding and comparing the applicability of electromembrane extraction (EME) and liquid-phase microextraction (LPME) is crucial for selecting an appropriate microextraction approach. In this work, EME and LPME based on supported liquid membranes were compared using biological samples, including whole blood, urine, saliva, and liver tissue. After optimization, efficient EME and LPME of clozapine from four biological samples were achieved. EME provided higher recovery and faster mass transfer for blood and liver tissue than LPME. These advantages were attributed to the electric field disrupting clozapine binding to interfering substances. For urine and saliva, EME demonstrated similar recoveries while achieving faster mass transfer rates. Finally, efficient EME and LPME were validated and evaluated combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The coefficient of determination of all methods was greater than 0.999, and all methods showed acceptable reproducibility (≤14%), accuracy (90%-110%), and matrix effect (85%-112%). For liver and blood with high viscosity and complex matrices, EME-LC-MS/MS provided better sensitivity than LPME-LC-MS/MS. The above results indicated that both EME and LPME could be used to isolate non-polar basic drugs from different biological samples, although EME demonstrated higher recovery rates for liver tissue and blood.

Molecularly imprinted polymers by reflux precipitation polymerization for selective solid-phase extraction of quinolone antibiotics from urine.

Molecularly imprinted polymers (MIPs) possess high specific cavities towards the template molecules, thus solid-phase extraction (SPE) based on MIPs using the target as the template has been widely used for selective extraction. However, the performance of SPE depends strongly on the shape and the distribution of the MIP sorbents, and rapid synthesis of MIPs with uniform particles remains a challenge. Our previous studies have shown that reflux precipitation polymerization (RPP) was a simple and rapid method for the synthesis of uniform MIPs. However, synthesis of MIPs by RPP for a group of targets using only one of the targets as the template has rarely been reported. In this work, MIPs with specific recognition capability for a group of quinolone antibiotics were synthesized for the first time via RPP with only ofloxacin as the template. The synthesized MIPs displayed good adsorption performance and selectivity (IF > 3.5) towards five quinolones, and subsequently were used as SPE adsorbents. Based on this MIPs-SPE, after systematic optimization of the SPE operation parameters during loading, washing and elution, an efficient and sensitive enough SPE method for separation and enrichment of the five quinolones in urine was developed and evaluated in combination with LC-MS/MS. The results showed that MIPs-SPE-LC-MS/MS has a good correlation (R2 ≥ 0.9961) in the linear range of 1-500 µg L-1. The limit of detection (LOD) and limit of quantification (LOQ) for the five quinolones were 0.10-0.14 µg L-1 and 0.32-0.48 µg L-1, respectively. In addition, the proposed method demonstrated good reproducibility (≤ 13 %) and high accuracy (92 %-113 %). We are confident that this method holds significant promise for the analysis of quinolones within the contexts of forensic medicine, epidemiology, and environmental chemistry.