Development and validation of LC-MS/MS method for the determination of cyproheptadine in several pharmaceutical syrup formulations

J Pharm Biomed Anal. 2009 Dec 5;50(5):1044-9. doi: 10.1016/j.jpba.2009.06.006. Epub 2009 Jun 12.

Abstract

A rapid and sensitive liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed and validated for the qualitative and quantitative assay of cyproheptadine (CP) in pharmaceutical samples. Diphenylpyraline hydrochloride (DPP) was used as an internal standard (IS). Two multiple reaction-monitoring (MRM) transitions for each analyte were observed: 288.1/96.1 and 288.1/191.2 for CP and 282.1/167.2 and 282.1/116.3 for DPP. The retention time of the drug was 7.29 min. The analytical method was successfully validated for linearity (1-100 ng/ml), intra-day precision, inter-day precision, and accuracy. The limit of detection (LOD) and limit of quantification (LOQ) were 0.86 and 0.98 ng/ml, respectively. The proposed method was applied to analyse the cyproheptadine content from seven different syrup formulations.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Calibration
  • Chemistry, Pharmaceutical / methods*
  • Chromatography, Liquid / methods*
  • Cyproheptadine / analysis*
  • Drug Stability
  • Food Contamination
  • Models, Chemical
  • Pharmaceutical Preparations / analysis*
  • Reproducibility of Results
  • Solvents / chemistry
  • Tandem Mass Spectrometry / methods*
  • Temperature
  • Time Factors

Substances

  • Pharmaceutical Preparations
  • Solvents
  • Cyproheptadine