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ISRN Analytical Chemistry
Volume 2013 (2013), Article ID 542516, 5 pages
http://dx.doi.org/10.1155/2013/542516
Research Article

Simple and Sensitive Methods for the Determination of 2-(4′-Chloromethyl phenyl) Benzonitrile and 2-(4′-Bromomethyl phenyl) Benzonitrile Contents in Valsartan Drug Substance by Gas Chromatography

1Aurobindo Pharma Limited Research Centre-II, Survey No. 71&72, Indrakaran Village, Sangareddy Mandal, Medak, Andhra Pradesh 502 329, India
2Department of Chemistry, Sri Krishnadevaraya University, Anantapur 515 003, India

Received 22 April 2013; Accepted 14 May 2013

Academic Editors: S. Babic, T. Bolanca, A. Niazi, and G. Vecchio

Copyright © 2013 G. Amarnatha Reddy et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

Simple and reliable gas chromatographic methods were developed, optimized, and validated for the determination of 2-(4′-chloromethyl phenyl) benzonitrile (2-CMPB) and 2-(4′-bromomethyl phenyl) benzonitrile (2-BMPB) contents in valsartan drug substance, using benzophenone as internal standard (IS). Efficient chromatographic separations were achieved on DB-1, 30 m length with 0.53 mm i.d., and 3 μm particle diameter column consists of 100% dimethyl polysiloxane as a stationary phase by passing helium as a carrier gas. The analytes were extracted in dichloromethane and monitored by flame ionization detector. The performance of these methods was assessed by evaluating specificity, precision, sensitivity, linearity, and accuracy. The limits of detection (LOD) and limits of quantification (LOQ) established for 2-CMPB are 0.10 μg mL−1 and 0.32 μg mL−1, respectively. For 2-BMPB, LOD is 0.31 μg mL−1 and LOQ is 0.95 μg mL−1. The average recoveries for 2-CMPB are in the range of 96.8% to 106.7% and for 2-BMPB (LOQ level) are 99.3%. The methods can be successfully applied for the routine analysis of valsartan drug substance.