Development of Ion Chromatography Method for Analysis of Organic Anions (Fumarate, Oxalate, Succinate, and Tartrate) in Single Chromatographic Conditions

Yarbagi Kaviraj

doi:10.3797/scipharm.1503-15

Abstract

A single organic counterion analysis method was developed by using an ion chromatography separation technique and conductivity detector. This allows the rapid characterization of an API to support clinical studies and to fulfil the regulatory requirements for the quantitation of fumarate, oxalate, succinate, and tartrate counterions in active pharmaceutical ingredients (quetiapine fumarate, escitalopram oxalate, sumatriptan succinate, and tolterodine tartrate). The method was developed by using the Metrohm Metrosep A Supp 1 (250 × 4.0 mm, 5.0 µm particle size) column with a mobile phase containing an isocratic mixture of solution A: 7.5 mM sodium carbonate and 2.0 mM sodium bicarbonate in Milli-Q water and solution B: acetonitrile. The flow rate was set at 1.0 mL/min and the run time was 25 minutes. The developed method was validated as per ICH guidelines, and the method parameters were chosen to ensure the spontaneous quantitation of all four anions. The method was validated for all four anions to demonstrate the applicability of this method to common anions present in various APIs.

Highlights

A salt is a “chemical compound comprising an assembly of cations and anions.” a pharmaceutical salt comprises an active pharmaceutical ingredient (API) that is molecular and either cationic or anionic and has a counterion that might be molecular or monatomic [1]
Various trials were performed for the method development of organic anion content in quetiapine fumarate, escitalopram oxalate, sumatriptan succinate, and tolterodine tartrate
The specificity of the developed ion-exchange chromatographic method was established in the presence of 11 anions and four active pharmaceutical ingredients (API), namely trifluoroacetic acid (TFA), chloride, nitrate, bromide, phosphate, sulphite, succinate, tartrate, sulphate, oxalate, fumarate and the APIs quetiapine, escitalopram, sumatriptan, and tolterodine

Summary

Introduction

A salt is a “chemical compound comprising an assembly of cations and anions.” a pharmaceutical salt comprises an active pharmaceutical ingredient (API) that is molecular and either cationic or anionic and has a counterion that might be molecular or monatomic [1]. A pharmaceutical salt comprises an active pharmaceutical ingredient (API) that is molecular and either cationic or anionic and has a counterion that might be molecular or monatomic [1]. The first is to demonstrate the quantification of an appropriate amount of anionic counterion in the salt, which is an important step in the characterization of an API [2, 3]. This work describes the development of chromatographic parameters and sample preparation procedures for a single method for the quantification of fumarate, oxalate, succinate, and tartrate by IC. Analytical grade sodium carbonate and sodium bicarbonate were purchased from S.D. Fine Chemicals, Mumbai, India. Analytical grade fumaric acid, oxalic acid, succinic acid, and tartaric acid were purchased from Qualigens Fine Chemicals, Mumbai, India. Quetiapine fumarate, escitalopram oxalate, sumatriptan succinate, and tolterodine tartrate were the APIs for research (Fig. 1), which were obtained from Dr Reddy’s Laboratories Ltd, Hyderabad, India

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Results

Conclusion