Five thiourea derivative ligands and their Ni2+ and Cu2+ complexes have been synthesized. The compounds were screened for their in vitro anti-bacterial activity using Gram-positive bacteria (two different standard strains of Staphylococcus aureus, Staphylococcus epidermidis, Enterococcus faecalis, Streptococcus pyogenes, Bacillus cereus) and Gram-negative bacteria (Esherichia coli, Pseudomonas aeruginosa, Enterobacter cloacae, Proteus vulgaris, Enterobacter aerogenes) and in vitro anti-yeast activity (Candida albicans, Candida krusei, Candida glabrata, Candida tropicalis, Candida parapsilosis). The minimum inhibitory concentration was determined for all ligands and their complexes. In vitro anti-yeast activity of both ligands and their metal complexes is greater than their in vitro anti-bacterial activity. The effect of the structure of the investigated compounds on the antimicrobial activity is discussed.
The feasibility of using a new and more versatile polymeric chiral surfactant, i.e., poly(sodium N-undecenoxy carbonyl-L-leucinate (poly-L-SUCL) is investigated for simultaneous enantioseparation and detection of eight structurally similar beta-blockers with tandem UV and MS detection. Three optimization approaches, i.e., direct infusion-MS, capillary zone electrophoresis-MS, and chiral micellar electrokinetic chromatography-mass spectrometry (CMEKC-MS), were investigated to optimize sheath liquid parameters, spray chamber parameters, and CMEKC separation parameters for maximum sensitivity and chiral resolution. Compared to unpolymerized micelle of L-SUCL, the use of micelle polymer (i.e., poly-L-SUCL) provided significantly higher separation efficiency, lower separation current, and higher detection sensitivity for CMEKC-ESI-MS of beta-blockers. It was also observed that, unlike monomeric L-SUCL, polymeric L-SUCL provided enantioseparation of all beta-blockers even at the lowest surfactant concentration (i.e., 5 mM poly-L-SUCL). Under optimum CMEKC and ESI-MS conditions (15 mM poly-L-SUCL, 25 mM each of NH4OAc and TEA (pH 8.0); 80% (v/v) methanol sheath liquid containing 40 mM NH4OAc (pH 8.0); sheath liquid flow rate, 5.0 microL/min; drying gas flow rate, 5 L/min; drying gas temperature, 200 degrees C; nebulizing pressure, 6 psi (0.414 bar); capillary voltage, +2.5 kV; fragmentor voltage, 85 V), baseline enantioseparation of eight beta-blockers was achieved by tandem UV (in approximately 30 min) and MS (in approximately 60 min) detection. Calibration curves for all beta-blockers were linear in the range of 0.01-0.6 mM for both CMEKC-UV and CMEKC-MS methods, but the later method provided better concentration limit of detection with similar RSD for migration time and peak areas. The CMEKC-ESI-MS method appears suitable for use as a routine procedure for high-throughput separation of beta-blockers with high sensitivity.
Electrokinetic chromatography (EKC) with poly(sodium undecylenic sulfate) (poly-SUS) is utilized to separate environmental pollutants such as 2−6-ring polycyclic aromatic hydrocarbons (PAHs). Parameters such as pH, concentration of polymeric surfactants, and the use of organic modifiers were investigated to follow the retention trends of PAHs. A baseline separation of all 16 PAHs in about 30 min, using 0.50% (w/v) of poly-SUS/12.5 mM sodium phosphate−borate buffer (pH 9.2) with 40% (v/v) acetonitrile, was possible for the first time in EKC by a single-surfactant system.
Open-tubular capillary electrochromatography (OT-CEC) is an alternative approach to conventional CEC. The primary advantage of OT-CEC is the elimination of problems associated with frits and silica particles in conventional CEC. This report is an investigation of the utility of using a polymeric surfactant (molecular micelle) for OT-CEC. In this approach, fused-silica capillaries coated with thin films of physically adsorbed charged polymers are developed by use of a polyelectrolyte multilayer (PEM) coating procedure. The PEM coating is constructed in situ by alternating rinses with positively and negatively charged polymers, where the negatively charged polymer is a molecular micelle. This can offer a number of advantages for separation of hydrophobic analytes. In this study, poly(diallyldimethylammonium chloride) was used as the cationic polymer and poly(sodium N-undecanoyl-L-glycinate) was used as the anionic polymer for PEM coating. The performance of the modified capillaries as a separation medium is evaluated by use of seven benzodiazepines as analytes. The run-to-run, day-to-day, week-to-week, and capillary-to-capillary reproducibilities of electroosmotic flow are very good with relative standard deviation values of less than 1% in all cases. In addition, the chromatographic performance of the monomeric form of the molecular micelle is compared for the separation of these analytes. The PEM-coated capillary was remarkably robust with more than 200 runs accomplished in this study. Strong stability against extreme pH values was also observed. The general utility of this approach is discussed in detail.
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