Journal of Pharmaceutics & Drug Delivery Research ISSN: 2325-9604

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Research Article, J Pharm Drug Deliv Res Vol: 5 Issue: 3

Application of an LC-MS/MS Method in Quantification of Hexyl Chloroformate Content in Dabigatran Etexilate Mesylate

Rakesh Kumar Yadav1*, Jayvant Harlikar1, Jaidatta Deshmukh1, Chetan M. Bhalgat1, Dipak Thange1, Hemant Birari1, Manish Gangrade1, Srinivas V Pullela1 and Vinod Acharya2
1Analytical R&D (API-IPD), Cipla Ltd, Vikhroli (W), Mumbai-400083, Maharashtra, India
2API-R&D Cipla Ltd, Vikhroli (W), Mumbai-400083, Maharashtra, India
Corresponding author : Rakesh Kumar Yadav
Analytical R&D (API-IPD), Cipla Ltd, Vikhroli (W), Mumbai-400083, Maharashtra, India
Tel: +91-8805223432
E-mail: [email protected], [email protected]
Received: July 01, 2016 Accepted: September 19, 2016 Published: September 22, 2016
Citation: Yadav RK, Harlikar J, Deshmukh J, Bhalgat CM, Thange D, et al. (2016) Application of an LC–MS/MS Method in Quantification of Hexyl Chloroformate Content in Dabigatran Etexilate Mesylate. J Pharm Drug Deliv Res 5:3. doi:10.4172/2325-9604.1000154

Abstract

 Application of an LC–MS/MS Method in Quantification of Hexyl Chloroformate Content in Dabigatran Etexilate Mesylate

Abstract

A selective and sensitive liquid chromatography–mass spectrometry (AB SCIEX QTRAP 5500) method was developed for quantitative determination of genotoxic impurity, hexyl chloroformate, in drug substance. The method was developed by derivatizing the hexyl chloroformate (HCF) to complex compound hexyl benzylcarbamate (HBC) by reaction with benzylamine. This method provided good sensitivity for quantification of hexyl chloroformate at a concentration of 10 ppm in 10 mg/mL DEM sample solution. The compounds were chromatographed under isocratic condition on poroshell EC-C18 (2.7 μm particle packed in 4.6 x 50 mm column) column with mobile phase of 0.1% v/v ammonium hydroxide in water (pH adjusted to 6 using acetic acid) and acetonitrile in ratio of 1:1 v/v at the flow rate of 1.0 ml/minute with triple quadrupole Q-Trap 5500 mass spectrometer operated in multiple reaction monitoring mode (MRM). To produce transition ion of 236/152 the molecular mass of 236(M+H) was used as molecular ion. Positive mode electro spray ionization (ESI) was employed as the ionization source. The developed method was validated in terms of specificity, limit of detection (LOD), limit of quantification (LOQ), linearity, precision, accuracy, and robustness. The LOD & LOQ were found at 2.1 and 4.2 ppm, respectively.

Keywords: Hexyl chloroformate; Dabigatran etexilate mesylate; Quantification; LC-MS/MS Q TRAP 5500; Method development; Validation

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