Use of Three-Dimensional Minimum  -Plots for Optimization of Mobile Phase Composition for RP-HPLC Separation of Sulfonamides

A sensitive and selective RP-HPLC method was developed and validated for the quantitative determination of trimazolin hydrochloride in nasal drops formulations. The mobile phase composition was water-acetonitrile (50:50, v/v) and the UV detection was carried out at 270 nm. Linearity range in the concentration range of 10 to 110 ?g cm-3. The method was tested and validated for various parameters according to ICH guidelines. The detection and quantization limits were found to be 1.45 and 4.8 ?g cm-3, respectively. The results demonstrated that the procedure for estimation of trimazolin hydrochloride in nasal drops formulations was accurate, precise and reproducible.

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IMPLICATIONS OF MOBILE PHASE COMPOSITION AND PH ON THE CHROMATOGRAPHIC SEPARATION OF AMITRIPTYLINE AND ITS METABOLITE NORTRIPTYLINE

International Journal of Pharmacy and Pharmaceutical Sciences ◽

10.22159/ijpps.2018v10i4.24817 ◽

2018 ◽

Vol 10 (4) ◽

pp. 132

Author(s):

Luana Mifsud Buhagiar ◽

Manuel Scorpiniti ◽

Nicolette Sammut Bartolo ◽

Janis Vella Szijj ◽

Victor Ferrito ◽

...

Keyword(s):

Liquid Chromatography ◽

Phase Composition ◽

Stationary Phase ◽

Mobile Phase ◽

Reversed Phase ◽

Organic Modifier ◽

Mobile Phase Composition ◽

Simple Method ◽

Column Temperature ◽

Rp Hplc

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.

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EFFECT OF MOBILE PHASE COMPOSITION AND pH ON HPLC SEPARATION OF RHIZOME OF POLYGONUM BISTORTA

Journal of Liquid Chromatography &amp Related Technologies ◽

10.1080/10826076.2011.615089 ◽

2012 ◽

Vol 35 (7) ◽

pp. 977-987 ◽

Cited By ~ 3

Author(s):

Azeem Intisar ◽

J. Boima Kiazolu ◽

Yun Wang ◽

Lingyi Zhang ◽

Weibing Zhang

Keyword(s):

Phase Composition ◽

Mobile Phase ◽

Hplc Separation ◽

Mobile Phase Composition

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Sequential Injection Chromatography with Monolithic Column for Phenothiazines Assay in Human Urine and Pharmaceutical Formulations

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190219143750 ◽

2020 ◽

Vol 16 (7) ◽

pp. 967-975

Author(s):

Abubakr M. Idris

Keyword(s):

Phase Composition ◽

Human Urine ◽

Mobile Phase ◽

Monolithic Column ◽

Pharmaceutical Formulations ◽

Pharmaceutical Formulation ◽

Assay Method ◽

Sequential Injection ◽

Mobile Phase Composition ◽

Sequential Injection Chromatography

Methods: Sequential injection chromatography (SIC) with monolithic column has been proposed with potential benefits for separation and quantification. Objective: To utilize SIC to develop a new assay method for the separation and quantification of some phenothiazines (promethazine, chlorpromazine and perphenazine) in human urine and synthetic pharmaceutical formulations. Methods: The 32 full-factorial design was adopted to study the effect of mobile phase composition on separation efficiency, retention time, peak height and baseline. The separation was conducted on a C18 monolithic column (100 × 4.6 mm) using a mobile phase composition of phosphate: acetonitrile:methanol (60:28:12) at pH 4.0. The detection was carried out using a miniaturized fiber optic spectrometer at 250 nm. Results: Satisfactory analytical features, including number of theoretical plates (1809-6232), peak symmetry (1.0-1.3), recovery (95.5-99.1% in pharmaceutical formulations and 91.6-94.7% in urine), intra-day precision (0.36-1.60% for pharmaceutical formulation and 2.96-3.67 for urine), inter-day precision (1.47-2.28% for pharmaceutical formulation), limits of detection (0.23-0.88 μg/ml) and limits of quantification (0.77-2.90 μg/ml), were obtained. Conclusion: The remarkable advantages of the proposed SIC method are the inexpensiveness in terms of instrumentation and reagent consumption.

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