This work relates to the preparation of novel and promising stationary phases containing inorganic-organic composites for capillary liquid and gas chromatography. A naturally occurring montmorillonite was introduced to polymethacrylate monoliths, then used under different conditions of GC and HPLC at the same time. The performance of the columns was evaluated for the separation of alkane and alkylbenzene series in GC and capillary HPLC, respectively. While the bare monoliths failed to separate the model analytes, montmorillonite-based polymethacrylate allowed a full separation of the mixtures with Rs≥1.42. The columns were applied for the determination of myrcene and limonene isomers in the peel extracts of some fruits using GC, and for the analysis of active ingredients including aspirin, vitamin-C, caffeine, and ibuprofen extracted from common drugs using capillary HPLC. In GC, fast separation was achieved in 1.0 min with Rs of 6.53. The columns exhibited the best efficiency for myrcene with 20,900 plates/m. Using the capillary HPLC columns, the active ingredients were resolved in 10 min with Rs≥5.72. The efficiency values located between 12,800-21,700 plates/m in all cases. The developed methods were found to be linear in the range of 0.10-10.0 and 0.20-180 μg/mL for GC and HPLC, respectively. In comparison with commercial columns, the results in GC methods reveal that, despite their much shorter length, the prepared columns proved a faster separation with higher efficiency and comparable detection limits and chromatographic resolution. The prepared HPLC capillaries exposed lower run times and detection limits with comparable efficiency and resolution, and consume fewer samples and mobile phase solvents. The results demonstrate that the montmorillonite-based polymethacrylate composites are applicable as stationary phases for routine analysis and quality control of important fields such as food and pharmaceutical samples.
Keywords: Column preparation; Monolith material; Montmorillonite; Polymethacrylate; Stationary phase.
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