scholarly journals Analysis of Some Biogenic Amines by Micellar Liquid Chromatography

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Irena Malinowska ◽  
Katarzyna E. Stępnik

Micellar liquid chromatography (MLC) with the use of high performance liquid chromatography (HPLC) was used to determine some physicochemical parameters of six biogenic amines: adrenaline, dopamine, octopamine, histamine, 2-phenylethylamine, and tyramine. In this paper, an influence of surfactant’s concentration and pH of the micellar mobile phase on the retention of the tested substances was examined. To determine the influence of surfactant’s concentration on the retention of the tested amines, buffered solutions (at pH 7.4) of ionic surfactant—sodium dodecyl sulfate SDS (at different concentrations) with acetonitrile as an organic modifier (0.8/0.2 v/v) were used as the micellar mobile phases. To determine the influence of pH of the micellar mobile phase on the retention, mobile phases contained buffered solutions (at different pH values) of sodium dodecyl sulfate SDS (at 0.1 M) with acetonitrile (0.8/0.2 v/v). The inverse of value of retention factor () versus concentration of micelles () relationships were examined. Other physicochemical parameters of solutes such as an association constant analyte—micelle ()—and partition coefficient of analyte between stationary phase and water (hydrophobicity descriptor) () were determined by the use of Foley’s equation.

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Danielle Cristina da Silva ◽  
Cláudio Celestino Oliveira

Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17α-ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v) ethanol, 3.0% (m/v) sodium dodecyl sulfate (SDS), and 0.02 mol·L−1 phosphate at pHs 7.0 and 8.0, respectively. The method is simple, selective, and fast, and the analytes were separated in 23.0 min. For extraction, 1000 mL of sample containing 2.0% (v/v) ethanol and 0.002 mol·L−1 citric acid at pH 2.50 was loaded through a 1000 mg of C18 cartridge. The analytes were eluted using 3.0 mL of ethanol, which were evaporated and redissolved in 0.5 mL of mobile phase. Concentration factors better than 1200, except amoxicillin (224), were obtained. The analytical curves were linear (R2 better than 0.992); LOD and LOQ n=10 presented values in the range of 0.019–0.247 and 0.058–0.752 mg·L−1, respectively. Recoveries of 99% were obtained, and the results are in agreement with those obtained by the comparative methods.


2015 ◽  
Vol 28 (2) ◽  
pp. 126-130
Author(s):  
Anna Petruczynik ◽  
Grzegorz Noster ◽  
Monika Waksmundzka-Hajnos

Abstract In this work, the effects of sodium dodecyl sulfate (SDS) concentrations on retention, separation selectivity, peak shapes and systems efficiency were investigated. Herein, the retention data for 11 alkaloids were determined on an RP18 silica column with mobile phases containing methanol as organic modifier, with acetate buffer at pH 3.5, and, subsequently, with the addition of sodium dodecyl sulfate (SDS). The results of this study indicate that the retention of alkaloids decreases with the increase of SDS concentration in the mobile phase. The increase of SDS concentration, however, leads to the significantly improvement of peak symmetry and the increase of theoretical plate number in all cases. The best system efficiency for most of the investigated alkaloids was obtained in a mobile phase containing 0.1 M SDS, while most symmetrical peaks were obtained through the addition of 0.3 M of SDS to the mobile phase.


2020 ◽  
Vol 18 (1) ◽  
pp. 377-390
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba

AbstractA stability-indicating hybrid micelle liquid chromatography accompanied by UV detection was developed for the simultaneous analysis of either paracetamol (PCA) or pseudoephedrine hydrochloride (PSU) with their synthetic impurities. Mixture I contains PCA with p-amino phenol and p-nitro phenol, while mixture II involves the estimation of PSU with benzaldehyde and benzoic acid. Both mixtures were separated using a C18 column that was thermostatically maintained at 40°C and operating under a flow rate of 1.5 mL/min, applying UV detection at 240 nm for mixture I and 220 nm for mixture II. In both cases, the mobile phase consisted of 0.1 M sodium dodecyl sulfate, acetonitrile, and triethylamine (90:10:0.3, v/v/v) and adjusted to pH 4 (mixture I) or pH 3.7 (mixture II) using 2.0 M O-phosphoric acid. The proposed method was validated and successfully applied to assay different pharmaceuticals containing PCA or PSU. Moreover, the stability-indicating nature of the proposed method was proved through applying photolytic degradation procedures for PCA.


2013 ◽  
Vol 96 (6) ◽  
pp. 1315-1324 ◽  
Author(s):  
Mohamed I Walash ◽  
Fathalla Belal ◽  
Nahed El-Enany ◽  
Manal Eid ◽  
Rania N El-Shaheny

Abstract A stability-indicating micellar liquid chromatography (MLC) method was developed and validated for the assay of floctafenine (FLF) in the presence of its degradation product and main metabolite, floctafenic acid (FLA). The analysis was carried out on a CLC Shim-Pack octyl silane (C8) column (150 × 4.6 mm id, 5 μm particle size) using a micellar mobile phase consisting of 0.15 M sodium dodecyl sulfate, 10% n-propanol, and 0.3% triethylamine in 0.02 M orthophosphoric acid (pH = 3). The mobile phase was pumped at a flow rate of 1.0 mL/min with UV detection at 360 nm. The method showed good linearity for FLF and FLA over the concentration ranges of 0.5–25.0 and 0.4–10.0 μg/mL, with LODs of 0.16 and 0.12 μg/mL, respectively. The developed method was successfully applied to the determination of FLF in commercial dispersible tablets, with mean recovery of 98.87 ± 1.37%. Also, the proposed method was specific for the analysis of FLF in presence of the co-formulated drug thiocolchicoside in laboratory-prepared tablets, with mean recovery of 100.50 ± 1.07%. Statistical comparison of the results obtained by the proposed MLC method with those obtained by a comparison method showed good agreement. Moreover, the method was extended to study the degradation behavior of FLF under different International Conference on Harmonization recommended conditions such as alkaline, acidic, oxidative, thermal, and photolytic. The method was further applied for direct determination of FLA as the main metabolite of FLF in human plasma without prior extraction steps, with mean recovery of 110.50 ± 6.5%.


2012 ◽  
Vol 2012 ◽  
pp. 1-5
Author(s):  
Maria Rambla-Alegre

Retention in micellar liquid chromatography is highly reproducible and can be modelled using empirical or mechanistic models with great accuracy to predict the retention changes when the mobile phase composition varies (surfactant and organic solvent concentrations), thus facilitating the optimisation of separation conditions. In addition, the different equilibria inside the column among the solute, the mobile phase, and the modified stationary phase by monomers of surfactant have been exhaustively studied. In a sequential strategy, the retention of the solutes is not known a priori, and each set of mobile phases is designed by taking into account the retention observed with previous eluents. By contrast, in an interpretative strategy, the experiments are designed before the optimization process and used to fit a model that will allow the prediction of the retention of each solute. This strategy is more efficient and reliable. The sequential strategy will be inadequate when several local and/or secondary maxima exist, as frequently occurs in chromatography, and may not give the best maximum, that is to say, the optimum. More often than not, the complexity of the mixtures of compounds studied and the relevant modification of their chromatographic behaviour when changing the mobile phase composition requires the use of computer-assisted simulations in MLC to follow the modifications in the chromatograms in detail. These simulations can be done with sound reliability thanks to the use of chemometrics tools.


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