Densitometric Determination of Embelin in Lysimachia punctata

JPC – Journal of Planar Chromatography – Modern TLC - Athin layer chromatographic method with densitometric UV detection at λ = 285 nm has been developed for quantification of...     

Simultaneous Determination of Cefuroxime Axetil and Cefuroxime in Pharmaceutical Preparations by Thin-Layer Chromatography and Densitometry

Summary Conditions have been established for identification and quantification of cefuroxime axetil and cefuroxime by thin-layer chromatography and densitometry. Good separation of these compounds was achieved on silica gel by use of chloroform–ethyl acetate–glacial acetic acid–water, 4:4:4:1 (v/v), as mobile phase. UV densitometry was used to detect spots on chromatograms. Under these conditions the limits of detection for cefuroxime axetil and cefuroxime were 40 ng and 30 ng, respectively. Recoveries of cefuroxime axetil and cefuroxime were 99.93% and 97.94%, respectively.     

Lipophilicity study of eight cephalosporins by reversed‐phase thin‐layer chromatographic method

The lipophilicity (R_M0) and specific hydrophobic surface area for the representatives of four generation cephalosporins have been determined by reversed‐phase thin‐layer chromatography, and the effect of different mobile‐phase modifiers (such as methanol, acetonitrile, acetone, 1,4‐dioxane and 2‐propanol) on the retention has been studied. The compounds studied showed typical retention behavior; their R_M values decreased linearly with increasing concentration of the organic modifier in the eluent. The linear correlations between the volume fraction of the organic solvent and the R_M values over a limited range were established for each solute, resulting in high values of correlation coefficients (>0.95 in most cases). R_M values were determined by various concentrations of organic modifier, and the correlation obtained was extrapolated to 0% of organic modifier. Chromatographically established logP (R_M0) parameters were compared with computationally calculated partition coefficients values (AClogP, ALOGP, KOWWIN, ALOGPs, XLOGP2, MLOGP and XLOGP3) and experimental octanol–water logP values (measured by the shake flask method). The received results demonstrate that RP‐TLC may be a good alternative technique for analytics in describing the lipophilic nature of investigated cephalosporins as well as the activity. Copyright © 2015 John Wiley & Sons, Ltd.     

Evaluation of a TLC Densitometric Method for Analysis of Azole Antifungal Agents

A new method for identification and quantitative determination of the azole antifungal agents; ketoconazole, bifonazole, fluconazole and itraconazole is described using TLC with densitometric detection. Validation of the method was carried out to confirm its precision (%RSD ranged between 1.31 and 3.45), recovery (99.7–102.4%) and linearity (r  = 0.99287–0.99722) within the concentration range under investigation. The experimental conditions obtained enable the method to be used for both qualitative and quantitative pharmaceutical analysis.

     

Separation,Identification, and Quantitative Analysis of the Epimers of Cefaclor by TLC-Densitometry

JPC – Journal of Planar Chromatography – Modern TLC - The epimers of cefaclor have been separated, identified, and analyzed quantitatively by TLC. The stationary phase was silica gel 60...     

Stability studies of clonazepam, diazepam, haloperidol, and doxepin with diverse polarities in an acidic environment

Stability of clonazepam, diazepam, haloperidol, and doxepin was determined in acidic solutions. In addition, determination of the kinetic and thermodynamic properties of this stability was carried out. Reaction rate constants (k), half-life times (t(0.1) and t(0.5)), and activation energy (Ea) were estimated for the drugs, which differed in polarity expressed with log P values. It was observed that estimated Ea values increased from 42.13 to 125.03 kJ/mol with an increase of lipophilicity (log P) beginning from the most hydrophilic drug (clonazepam, 2.70 log P) to the most lipophilic drug (doxepin, 4.10 log P). All degradation products were studied using an HPLC/electrospray ionization-MS technique in the positive ionization mode.     

Separation and determination of rofecoxib and its degradation products by TLC chromatography

A thin layer chromatography with densitometry method for the determination of rofecoxib and degradation products is described. The chromatographic separation was performed on silica gel TLC plates as a stationary phase and chloroform-acetone-toluene-glacial acetic acid (12: 5: 2: 0.1, v/v/v/v) as a mobile phase. Densitimetric detection was carried out at 256 nm. The method is of high sensitivity and low LOD and LOQ: from 0.35 μg/spot to 1.05 μg/spot. The recovery was satisfactory at 98.62%. In addition, the stability of rofecoxib in solutions was investigated, including an effect of solution pH, temperature and incubation time. The method is rapid, easy and selective, particularly for the analysis of rofecoxib formulations. The article is published in the original.     

Determination of gliclazide in pharmaceutical preparations by capillary gas chromatography with cool on-column injection and elimination of the matrix effect.

Conditions were established for the identification and quantitation of gliclazide in pharmaceutical preparations by capillary gas chromatography with flame ionization detection and cool on-column injection. Gliclazide was extracted with methanol and, after filtration, assayed on a (25 m x 0.25 mm id, 0.2 microm film thickness) CP-WAX 58 (FFAP)-CB WCOT fused silica column. Because the available preparations were of various origins and, therefore, could differ in auxiliary substances and their qualitative parameters, the influence of the matrix constituents on the analytical results was taken into account. Good separation conditions were established for the developed method. The retention time of gliclazide is about 36 min and differs from the retention times of the internal standard (approximately 29 min) and additional peaks present in chromatograms (20-26 min), which were assigned to matrix constituents. The recoveries of gliclozide were high and reached 96.5%. The developed method is characterized by selectivity and precision (relative standard deviation 0.38-1.26%), a wide range of linearity (0.1-10.0 mg/mL), and a limit of detection of 30 ng. In addition, the results of chromatographic analyses calculated in 3 ways were compared with those obtained by UV spectrophotometry. The suggested technique of cool on-column injection, in contrast with split-splitless injection (used in preliminary investigations), reduces to a minimum the possibility of thermal decomposition of gliclazide.     

Quality assessment for tramadol in pharmaceutical preparations with thin layer chromatography and densitometry

Research studies have been carried out to develop a chromatographic and densitometric method suitable for identification and determination of tramadol and impurities. In addition, the stability of tramadol in solutions was investigated, including an effect of solution pH, temperature and incubation time. In the first instance the conditions for identification and quantitative determination of tramadol and impurities in pharmaceutical preparations were established. The separation was performed on silica gel-coated chromatographic plates (HPTLC) using two mobile phases: (I) chloroform-methanol-glacial acetic acid (9:2:0.1, v/v/v); (II) chloroform-toluene-ethanol (9:8:1, v/v/v). The UV densitometry was carried out at lambda = 270 nm. The developed method is of high sensitivity and low detection and determination limits ranging from 0.044 to 0.35 microg. For individual constituents the recovery ranges from 93.23 to 99.66%. The next step was to evaluate the stability of tramadol and determine a method of decomposition under various experimental conditions. It was found that tramadol decomposes in various ways in acidic and basic environments producing (1RS)-[2-(3-methoxyphenyl)cyclohex-2-enyl]-N,N-dimethylmethanamine (imp. B) and (1RS, 2RS)-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol (imp. cis-T) or imp. cis-T, respectively.     

Reversed-phase high-performance liquid chromatography determination of selected phenolic acids in propolis concentrates in terms of standardization for drug manufacturing purposes

A reversed-phase high-performance liquid chromatography method with gradient elution was developed for the determination of the caffeic, p-coumaric, and ferulic acids in propolis concentrates. Solid-phase extraction on an RP18 column was applied for preliminary purification, and chromatographic separation was performed on 100 RP18e Lichrospher column of particle size 5 microm. The mobile phase was obtained by mixing in appropriate ratios 0.03 mM NaH2PO4, acidified with H3PO4 up to pH = 3.0, with acetonitrile to obtain a gradient in the elution process. Spectrophotometric detection was conducted at 320 nm. Under the established conditions, the method featured high sensitivity, good precision, and comparability of results, as proven by method validation and statistical analysis of the obtained results. The limits of detection were 0.315, 0.325, and 0.695 microg/mL for caffeic, p-coumaric, and ferulic acids, respectively. The corresponding recovery values were 98.14, 101.05, and 99.42% and the linearity ranges from 1.31 to 99.18 microg/mL, 1.52 to 119.16 microg/mL, and 2.42 to 184.14 microg/mL. The precision of the method was expresed by relative standard deviation values that did not exceed 3%. It was also shown that the propolis concentrates under examination had similar antibacterial activity against Staphylococcus aureus ranging from 119.8 to 124.3 microg/mL, contrary to model mixtures that showed no antibacterial activity.