Vol. 5 (03) pp. 1726-1733 DOI: 10.21474/IJAR01/3685

DETERMINATION OF RESIDUAL SOLVENTS IN NEOSTIGMINE METHYLSULFATE BY HEADSPACE GAS CHROMATOGRAPHY.

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  • Sir Sayyed College of Arts, Commerce and Science, P.G. Department of Chemistry, Roshangate, Aurangabad, 431001 Maharashtra, India.
  • Indoco Remedies Limited, Analytical research & development department, Navimumbai, 400701, Maharashtra, India.
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Abstract

A static headspace gas chromatographic (GC-HS) method is developed for quantitative determination of residual organic solvents such as acetone, ethyl acetate and acetonitrile used in the synthesis of Neostigmine Methylsulfate. Separation was achieved on capillary column DB-624 of length 30 m having internal diameter 0.32 mm and 1.8 ?m film thickness using a Flame ionization detector with gradient column oven temperature program. The headspace condition was optimized with the vial equilibration temperature of 100°C and time at 30 min. The injection was carried out in split mode, with a split ratio of 10:1. N-methyl-2-pyrrolidone is selected as a diluent to obtain good sensitivity along with the recovery. Analytical method validation was performed within the requirements of ICH validation guidelines Q2 (R1). System suitability parameter set with tailing factor, theoretical plate and relative standard deviation as required with various pharmacopoeias are checked. Limits of detection and quantitation, precision, linearity and accuracy along with robustness are performed, and acceptable results are obtained. The proposed developed method is demonstrated to be simple, sensitive, linear, accurate and robust, hence can be used to determine the residual organic solvents in Neostigmine methylsulfate drug substance.

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How to Cite This Article

Sayyed Hussain, Amit Gosar and Tabrez Shaikh. (2017); DETERMINATION OF RESIDUAL SOLVENTS IN NEOSTIGMINE METHYLSULFATE BY HEADSPACE GAS CHROMATOGRAPHY., Int. J. of Adv. Res., 5 (03), 1726-1733, ISSN 2320-5407. DOI: https://doi.org/10.21474/IJAR01/3685

Corresponding Author

TABREZ SHAIKH
Sir Sayyed College of Arts, Commerce and Science, P.G. Department of Chemistry, Roshangate, Aurangabad, 431001 Maharashtra, India
Creative Commons Attribution 4.0 This work is licensed under a Creative Commons Attribution 4.0 International License.