Authors:Ł. Komsta, R. Skibiński, A. Gumieniczek, and A. Wojnar
The thin-layer chromatographic (TLC) retention of 35 model compounds has been investigated with ten screening mobile phases on six normal-phase and seven reversed-phase adsorbents. The retention factors formed two cubes with dimensions 35 × 10 × 6 and 35 × 10 × 7, respectively, which enabled three-way analysis by PARAFAC. A one-component PARAFAC model was optimum in both cases and two-component models performed worse. The one-component model explained 78.8% of the variance in normal-phase chromatography and 94.2% of the variance in reversed-phase chromatography. These results showed that the major variability of the retention factor (RF) can be modelled as the product of three factors related to the substance itself, the mobile phase, and the adsorbent. RF modelling was substantially better than using k or RM (rate mobility) values.
Authors:T. W. Inglot, A. Gumieniczek, Ł. Komsta, and R. Związek
Comparison of classical densitometry, video-scanning, and capillary electrophoresis was performed for determination of angiotensin II receptor antagonist, valsartan, and calcium channels blocker, amlodipine, in a combined dosage form. Thin layer chromatography was performed on RP8F254 TLC plates with a mobile phase consisting of acetonitrile-phosphate buffer at pH 9.0 (5:5, v/v) and temperature 20 °C. Densitometry was done in the reflectance mode at 217 nm for valsartan and in the absorbance mode at 370 nm for amlodipine. Video-scanning was elaborated at 254 and 366 nm for valsartan and amlodipine, respectively. For chromatographic analysis, calibration plots were constructed in the range of 0.4–2.8 μg per spot for valsartan and 0.02–0.14 μg per spot for amlodipine. Capillary electrophoresis (CE) was performed using a 75 μm × 94 cm fused silica capillary (72 cm effective length), 0.01 mol L−1 borate buffer at pH 8.0, 20 kV voltage, 30 °C temperature, hydrodynamic injection (10 mbar, 6 s) and UV detection at 237 nm. Calibration plots were constructed in the range of 0.1–0.6 mg mL−1 for valsartan and 0.005–0.03 mg mL−1 for amlodipine. All methods were validated in respect to robustness, specificity, stability, linearity, precision, and accuracy. Generally, statistical comparison between the methods did not show significant differences so all procedures are suitable for pharmaceutical analysis.
Authors:E. Blicharska, Ł. Komsta, R. Kocjan, A. Gumieniczek, A. Kloc, and J. Kaźmierczak
The paper discusses a possibility to grow seeds on solutions of microelements and application of sprouts enriched in such a way as an alternative to commercial dietary supplements. It contains a short review of the approaches reported till now and a systematic experimental study, carried on the most frequently used seeds (Lens culinaris, Helianthus annuus, Vigna radiata, Glycine max, and Lepidium sativum).Seven metals (Fe, Cu, Zn, Ni, Co, Cd, and Mn) were studied. Seeds were grown on cellulose in 20°C temperature using deionized water enriched with metals in concentrations: 100, 50, 25, 12.5, 6.25, and 3.125 mg/L in a period of 4 days. The reference samples were the seeds grown on pure deionized water. Sprouts were mineralized by microwave radiation, and the metal content was quantified by ion chromatography with on-line post-column derivatization and spectrophotometric detection.The conclusions can be treated as general recommendations, which seeds should be grown and what concentrations of metals in solutions should be applied to provide good enrichment and to avoid risk of microelement overdose.