Estimation of lipophilicity and design of new 17β-carboxamide glucocorticoids using RP-HPLC and quantitative structure-retention relationships analysis

Eight 17β-carboxamide glucocorticoids with local anti-inflammatory activity were selected and their retention behavior tested in six RP-HPLC systems (I–VI). logkw, a, and φ0 parameters were calculated and correlation with previously determined logPo/w values was examined. RP-HPLC system IV, which consisted of cyano column and methanol–water mobile phases (50:50, 60:40, 70:30, and 80:20, v/v), was selected as the most reliable for lipophilicity prediction and used for the analysis of chromatographic behavior of remaining fourteen 17β-carboxamide glucocorticoids. Quantitative structure-retention relationships analysis was performed and PLS(logkw) model was selected as the most statistically significant. On the basis of selected model and interpretation of corresponding descriptors, new derivatives with higher logkw values and higher expected lipophilicity were designed.

Determination of Ardacin in Various Silage Feed Diets by a Rapid Liquid Chromatographic Assay

A method is presented for the detection and quantitation of Ardacin in silage feed diets by liquid chromatography, using a cyano column and an acetonitrile–methanol water mobile phase modified with trifluoroacetic acid. This method includes comprehensive procedures for extracting Ardacin from various silage feed formulations, cleaning up the extracted sample by using solid-phase extractions, and analyzing the eluted solid-phase extract with a suitable liquid chromatographic system. Ardacin was extracted from the silage feed formulations with 50% acetonitrile and 50% 0.1 M KOH. The extract was cleaned up with a wide-pore butyl solidphase extraction cartridge. The sample extract was chromatographed and quantified at 220 nm, using an external method of calculation. Recoveries of the medicated silage feed formulation ranged from 72.1 ± 1.7% to 109.1 ± 2.4%, depending on the sites and types of formulation analyzed.

Detection and Confirmation of Cocaine and Cocaethylene in Serum Emergency Toxicology Specimens

We report the performance of a liquid chromatography (LC) assay for detection and confirmation of cocaine and cocaethylene in serum. A photodiode array (PDA) detector monitors the cyano column effluent at 230 nm for analyte detection. Confirmation of a peak's identity is performed by use of only the 226-254-nm segment of the spectra rather than a broader range such as 210-340 nm. Use of the narrower range improves the assay's sensitivity by almost 10-fold. Analyte values of 10 micrograms/L are confirmed routinely. Intra-assay imprecision at 100, 20, and 10 micrograms/L for cocaine is 5.1%, 5.7%, and 6.6% (CV), respectively. Absolute recovery of the analytes exceeds 80%. In a split-sample study (33 positives and 74 negatives), each of this method's cocaine findings were confirmed. Cocaethylene was found in 15 of these samples. A complete chromatogram can be available 15 min after the start of the procedure. The method's focus on the active drug (rather than urinary metabolites) and its ability to detect and confirm many other drugs make it well suited for emergency toxicology testing.