• SUNNY GRACE GODE Department of Pharmacy, University College of Technology, Osmania University, Hyderabad, Telangana State India
  • VIJAYA LAKSHMI G. Department of Chemistry, Osmania University College for Women, Koti 500095, Hyderabad, Telangana State India



Netupitant, Residual Solvents, HeadSpace Gas Chromatography, International Conference on Harmonization.


Objective: Residual solvents are undesirable components present in Active Pharmaceutical Ingredients (API), excipients, or drug products. To meet the specific quality-based requirements, the presence of these solvents in pharmaceutical products should be monitored to ensure their safety. The main objective of this work is to develop a new method for the determination of residual solvents in netupitant API by an HS-GC method with an FID detector.

Methods: An automated headspace GC method has been developed and validated for the estimation of the residual solvents- N-methyl pyrrolidine, xylene, toluene, and N, N Dimethylacetamide in netupitant API. The samples were dissolved in dimethyl sulfoxide and

the equilibrium headspace gas was formed at 80℃ which was analyzed using a DB-624

column (30m*0.53mm, 3.00µm) with injector and detector temperature set at 160℃ and 230℃ respectively. The initial oven temperature was set at 60℃ for 5mins and programmed at a rate of 10℃/min to the final temperature of 150℃, with a hold time of 5mins by maintaining the flow rate of 4.0ml/min with a split ratio of 1:10, and total run time of 20mins. Nitrogen was used as carrier gas. The method developed was validated as per International Conference for Harmonization (ICH) guidelines for repeatability, linearity, range, ruggedness, detection limit, quantification limit, and recovery studies.

Results: The linearity range selected was 50-350µg/ml and the correlation coefficient(γ2) values for all the solvents were found to be >0.99; recovery studies values were in a range of 90-110% and %RSD values were also found to be not more than 10 for the solvents.

Conclusion: A novel, accurate, sensitive, and simple method was described for estimating residual solvents in Netupitant API by Headspace Gas Chromatography (HS-GC) coupled with a Flame Ionization Detector (FID). Excellent results have been observed for all the validated parameters with good peak resolution and lesser retention times.


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How to Cite

GODE, S. G., and V. LAKSHMI G. “ESTIMATION OF RESIDUAL SOLVENTS IN NETUPITANT API BY HEADSPACE GAS CHROMATOGRAPHY”. International Journal of Pharmacy and Pharmaceutical Sciences, vol. 13, no. 11, Sept. 2021, doi:10.22159/ijpps.2021v13i11.42781.



Original Article(s)