Efficiency enhancements in micellar liquid chromatography through selection of stationary phase and mobile phase organic modifier

2021 ◽  
Author(s):  
David Paul Thomas
1989 ◽  
Vol 61 (13) ◽  
pp. 1353-1358 ◽  
Author(s):  
Michael F. Borgerding ◽  
Willie L. Hinze ◽  
Larry D. Stafford ◽  
George W. Fulp ◽  
William C. Hamlin

2021 ◽  
Vol 08 ◽  
Author(s):  
Purushottam Sutar ◽  
Pravin Khedkar ◽  
Ganesh Chaturbhuj

Background: Sulfated Polyborate, a novel inorganic material primarily designed as a catalyst, has shown properties such as high solubility in organic solvents, low U.V. cut-off, and pKa ≈2.0, which suggests its potential as a mobile phase buffer for reverse-phase liquid chromatography. Objective: This study aims to substantiate the role of Sulfated Polyborate as mobile phase buffer for reverse-phase liquid chromatographic analysis of basic drugs with high pKa values viz. Bisoprolol fumarate, Timolol maleate, Verapamil hydrochloride, and Carvedilol. Methods: Solubilities, U.V. cut-offs, and pKa of Sulfated Polyborate was first experimentally confirmed. The behaviour of Sulfated Polyborate as mobile phase buffer at pH 3.0 was ascertained by varying the buffer concentration, flow rates, and percent organic modifier for elution of the four basic drugs on a non-end capped octyl silyl (C8) column. Similarly, the study was performed with KH2PO4 as a reference buffer. The column performance and conductometric measurements ascertained the impact of Sulfated Polyborate on the stationary phase. Results: Sulfated Polyborate and KH2PO4 buffers showed correlation coefficients of 0.99 and 1.00 for analyte retention factors for variation of buffer concentration and organic modifier composition, respectively. Peak symmetries and the number of theoretical plates were improved from > 2.0 to < 2.0 and ≈1000 to ≈3000, respectively, for Variation in buffer concentrations. Similar Van Deemter plots indicated equivalency of Sulfated Polyborate and KH2PO4 buffers. The column performance and conductometric measurements depicted no adsorption on the stationary phase. Conclusion: The present study demonstrates Sulfated Polyborate as a novel buffer for analytes with higher pKa on reverse-phase liquid chromatography.


Author(s):  
Luana Mifsud Buhagiar ◽  
Manuel Scorpiniti ◽  
Nicolette Sammut Bartolo ◽  
Janis Vella Szijj ◽  
Victor Ferrito ◽  
...  

Objective: Separation of tricyclic compounds sets the keystone for determining parent drug to metabolite concentration ratios and analysing impurities. The combined effects of acetonitrile composition and pH of the mobile phase on the separation of amitriptyline and nortriptyline by reversed-phase high-performance liquid chromatography (RP-HPLC) are presented.Methods: A series of RP-HPLC triplicate runs were carried out using acetonitrile and a phosphate buffer as the mobile phase and a Kinetex® C18 LC Column as the stationary phase using an Agilent 1260 Infinity Series® II liquid chromatography system with UV/visible detection. The stationary phase, column temperature, injection volume and flow rate were kept unchanged during analysis. Mobile phase composition and pH were varied to observe impact on peak shape, resolution and retention time, taking into consideration green analytical chemistry aspects.Results: Optimal chromatographic outcomes were achieved when using the mobile phase made up of 35% acetonitrile and 65% buffer at a pH of 5.6. These conditions resulted in nortriptyline and amitriptyline eluting at 4.66 min and 5.92 min respectively. Increasing the organic modifier content of the mobile phase to 40% completed separation within a run time of 4 min with comparable resolution. The 2 min gained by increasing 5% acetonitrile may not be justified due to potential implications on greening laboratory practices.Conclusion: Reversed-phase chromatography embodies a simple method for the separation of compounds that are similar in structure. Attuning the percentage of organic modifier and buffer pH provides acceptable retention times, without compromising resolution between neighbouring peaks.


The Analyst ◽  
1992 ◽  
Vol 117 (5) ◽  
pp. 831-837 ◽  
Author(s):  
María José Medina Hernández ◽  
María Celia García Alvarez-coque

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.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Magda T. Martins ◽  
Clésio S. Paim ◽  
Martin Steppe

Liquid chromatography (LC) and ultraviolet spectrophotometric (UV) methods for lamotrigine (LTG) determination were validated. The LC separation was achieved on an ACE RP-18 as stationary phase and 0.3% triethylamine in water (v/v) pH 4.0 : methanol (62 : 38, v/v) as mobile phase. Detection was achieved with a photodiode array at 279 nm. The detection response for LTG was linear (). The specificity and stability were proved using stress conditions. The CV (%) values for intraday and interday precision were less than 2.0%. The method was accurate and robust. The -student test proved that the LC and UV methods are interchangeable.


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