Determination of Azide and Bromide Ions by Direct Detection Using Capillary Electrophoresis

Author： Ram Reddy G. V. Praveen Kumar A. Venkateswara Reddy B. Sreeramulu J. Park Jung Hug

ISSN： 1082-6076

Source： Journal of Liquid Chromatography & Related Technologies, Vol.32, Iss.19, 2009-01, pp. : 2866-2878

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Abstract

The purpose of the present work was the development and validation of a simple, rapid, sensitive, and reliable method for the direct determinations of azide and bromide anions in valsartan and baclofen samples, respectively, based on capillary electrophoresis. Azide and bromide ions were determined using nitrate as an internal standard. Azide and nitrate were separated using a fused silica capillary column of total length 64.5 cm × 50 µm, and bromide and nitrate by a 104 cm × 50 µm capillary column. The background electrolyte was an inorganic anion buffer of pH 7.7, and UV detection at 245 nm was used for the determination. The detection limits for azide and bromide ions were 0.5 and 0.3 µg mL-1, respectively, with S/N ratios of less than 3.0 and the quantitation limits were 1.5 and 1.0 µg mL-1, respectively, with S/N ratios of less than 10.9. Excellent linearity was observed in the range from 5 - 30 µg mL-1 and 1 - 15 µg mL-1, for azide and bromide ions, respectively. Quantitative imprecision in intra-day (n = 5) and inter-day (n = 5) experiments was always within R.S.D. of <5%. Recovery was quantitative throughout the range of linearity of the method. Mean recovery values were ranging from 97.7 to 99.8% for both anions. The method was applied for the determination of azide and bromide contents in the batch samples of valsartan and baclofen, respectively. The developed method was validated in accordance with the ICH guidelines and proved to be suitable for its intended use.