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Detection And Quantification Of N-Ethyl-3-Chloro Pyrrolidine And Diphenyl Acetonitrile In Doxapram Hydrochloride Drug Substances Using Gas Chromatography Coupled With Mass Spectrometry Technique
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| Author:
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KOMALI SIVAPRASAD, VARDHANI DEVI DUGGIRALA PARVATHA VENKATA, KAPAVARAPU MARUTHIVENKATANARAYANARAO, PULIPAKASHYAMALA
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| Abstract:
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A gas chromatography with mass spectrometric method has been established and verified for the detection and quantitative analysis of two residual solvents in the drug substance, doxapram hydrochloride. The method was completely validated for two solvents, N-ethyl-3-chloro pyrrolidine and diphenyl acetonitrile. The proposed method uses a silica capillary column (DB 5MS, 30 m × 0.32 mm i.d., 0.25 µm thickness film) with oven temperature plan: hold the temperature at 50 °C for 3 min, then elevated to 220 °C at a rate of 20 °C/min and held there for 4 min followed by a raise to 280 °C temperature at a rate of 40 °C/min and held there for 13 min. The total run time is 29 min. Calibration lines for N-ethyl-3-chloro pyrrolidine and diphenyl acetonitrile were linear within the range of 0.25 ppm to 0.75 ppm and 0.032 ppm to 0.75 ppm, respectively. The relative standard deviations for N-ethyl-3-chloro pyrrolidine and diphenyl acetonitrile were smaller than 15%. The percent recoveries were 95.627% to 110.385% and 95.793% to 99.126% for N-ethyl-3-chloro pyrrolidine and diphenyl acetonitrile. The gas chromatography method developed will allow screening of doxapram hydrochloride drug substances for the presence of N-ethyl-3-chloro pyrrolidine and diphenyl acetonitrile.
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| Keyword:
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Doxapram hydrochloride, N-ethyl-3-chloro pyrrolidine, Diphenyl acetonitrile, Gas chromatography, Mass spectrometer, Analysis
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| EOI:
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| DOI:
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https://doi.org/10.31838/ijpr/2021.13.02.021
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| Download:
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