scholarly journals Retention behavior of selected alkaloids in Reversed Phase micellar chromatographic systems

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.

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.


2001 ◽  
Vol 84 (6) ◽  
pp. 1687-1694 ◽  
Author(s):  
Mayte Gil-Agustí ◽  
Llorenç Monferrer-Pons ◽  
Josep Esteve-Romero ◽  
María Celia García-Alvarez-Coque

Abstract A reversed-phase liquid chromatographic procedure with a micellar mobile phase of sodium dodecyl sulfate (SDS), containing a small amount of pentanol, was developed for the control of 7 antihistamines of diverse action in pharmaceutical preparations (tablets, capsules, powders, solutions, and syrups): azatadine, carbinoxamine, cyclizine, cyproheptadine, diphenhydramine, doxylamine, and tripelennamine. The retention times of the drugs were <9 min with a mobile phase of 0.15M SDS–6% (v/v) pentanol. The recoveries with respect to the declared compositions were in the range of 93–110%, and the intra- and interday repeatabilities and interday reproducibility were <1.2%. The results were similar to those obtained with a conventional 60 + 40 (v/v) methanol–water mixture, with the advantage of reduced toxicity, flammability, environmental impact, and cost of the micellar-pentanol solutions. The lower risk of evaporation of the organic solvent dissolved in the micellar solutions also increased the stability of the mobile phase.


Chemija ◽  
2018 ◽  
Vol 29 (4) ◽  
Author(s):  
Andrius Žilionis

Sodium dodecyl sulfate (SDS) is a widely used detergent for protein denaturation and solubilization. However, application of SDS in the sample preparation for the liquid chromatographic-mass spectrometric analysis is limited because commonly used SDS concentrations interfere with reversed phase liquid chromatography and electrospray ionization mass spectrometry. In order to analyse SDS pretreated proteins by the above-mentioned methods SDS must be completely removed or its concentration must be lowered to less than 0.01%. In this work we present a comparison of different SDS removal strategies based on SDS ultrafiltration, protein precipitation and SDS precipitation methods. Every strategy was optimized so that the initial 4% SDS concentration was lowered to less than 0.01% and the initial sample volume remained unchanged. The modified Mukerjee’s photometric method was used for the SDS quantitation in the presence of model protein bovine serum albumin and the recovery of model protein was evaluated using reversed phase ultra performance liquid chromatography. The main advantages and drawbacks of every strategy are discussed.


1994 ◽  
Vol 77 (1) ◽  
pp. 41-45 ◽  
Author(s):  
William A Moats

Abstract A method is described for determination of am-piciitin and amoxicillin in milk by using an automated liquid chromatographic (LC) cleanup. Milk was deproteinated by adding tetraethylammonium chloride solution and acetonitrile. The filtrate was concentrated by evaporation, filtered, and loaded into a 4 mL autosampler vial. For LC cleanup, a Waters W1SP 712 autosampler, a Varian 9010 pump, a Supelcosil LC-18 column, and an ISCO FOXY fraction collector were used. The cleanup program, where A is 0.01 M KH2PO4 and B is acetonitrile, was 100A + OB for 0-3 min and then 70A + 30B for 24 min. Sample concentrate (2 mL) was loaded onto the column for cleanup. Fractions containing amoxicillin and ampicillin were collected, partially acidified, and concentrated to 1 mL. Analysis was done on the LC-18 column, with a mobile phase of 0.015M H3PO4–{0.0075M sodium dodecyl sulfate-acetonitrile (70 + 30)] for amoxicillin and 0.0067M H3PO4–0.0033M KH2PO4–[0.005M sodium dodecyl sulfate–acetonitrile (67 + 33)] for ampicillin. Recoveries were generally 80–90% at a concentration range of 1–0.01 ppm, with a detection limit of 2–5 ppb. By collecting appropriate fractions, the method can be applied to the determination of any amphoteric β-lactam.


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