Identification of the Organic Volatile Impurities in Telmisartan Active Pharmaceutical Ingredient and Its Pharmaceutical dosage forms by using Head Space Gas Chromatography Technique

Residual solvents in pharmaceutical samples are monitored using gas chromatography with head space. Based on good manufacturing practices, measuring residual solvents is mandatory for the release testing of all active pharmaceutical ingredients (API). The analysis of residual organic solvents (methanol, acetone, cyclohexane, dichloromethane, toluene) in Omeprazole, an active pharmaceutical ingredient was investigated. Omeprazole is a potent reversible inhibitor of the gastric proton pump H+/K+-ATPase. The Head space gas chromatography (HSGC) method described in this investigation utilized a SPB TM-624, Supelco, 30 m long x 0.25 mm internal diameter, 1.4µm-thick column. Since Omeprazole is a thermally labile compound, the selection of the proper injector temperature is critical to the success of the analysis. The injector temperature was set at 170ºC to prevent degradation. The initial oven temperature was set at 40ºC for 12 min and programmed at a rate of 10ºC min-1 to a final temperature of 220ºC for 5 min. Nitrogen was used as a carrier gas. The sample solvent selected was N,N-dimethylacetamide. The method was validated to be specific, linear, precise, sensitive, rugged and showed excellent recovery.

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DEVELOPMENT AND VALIDATION OF A GAS CHROMATOGRAPHY HEADSPACE METHOD FOR THE SIMULTANEOUS QUANTIFICATION OF SIX ORGANIC VOLATILE IMPURITIES IN SUMATRIPTAN SUCCINATEAPI AND ITS PHARMACEUTICAL DOSAGE FORMS

Asian Journal of Pharmaceutical and Clinical Research ◽

10.22159/ajpcr.2020.v13i5.37260 ◽

2020 ◽

pp. 210-218

Author(s):

KRISHNA KISHORE J ◽

PRASADA RAO K

Keyword(s):

Gas Chromatography ◽

Dosage Forms ◽

Flame Ionization Detector ◽

Solution Stability ◽

Ionization Detector ◽

Pharmaceutical Dosage Forms ◽

Sumatriptan Succinate ◽

Simultaneous Quantification ◽

Flame Ionization ◽

Volatile Impurities

Objective: The main aim of this study, to develop a validated analytical method for simultaneous quantification of six organic volatile impurities (OVI) in sumatriptan succinate active pharmaceutical ingredients (API) and its pharmaceutical dosage forms by headspace (HS)-gas chromatography (GC). Methods: The method development and its validation were performed on a Shimadzu GC-2010 GC system equipped with a flame ionization detector and Teledynetekmar HT3TM HS analyzer. The method involved a thermal gradient elution of six OVI present in sumatriptan succinate API. DB-624, 30 m×0.53 mm, 3.0 μ column is used as a stationary phase and nitrogen gas is used as a carrier gas. The flow rate was 2.8 mL/min and the flame ionization detector temperature is 260°C. Results: The correlation coefficient (r2) was not <0.99 at the limit of quantification (LOQ) to 150%. The limit of detection obtained for methanol, acetone, isopropyl alcohol, dichloromethane, benzene, and toluene was found 18.4, 8.8, 5.5, 4.3, 0.04, and 4.2 ppm. The LOQ obtained was 55.8, 26.8, 16.6, 13.0, 0.1, and 12.6 ppm. Accuracy results were obtained from 85 to 115% for six OVI’s. Furthermore, verified precision, ruggedness, robustness, solution stability, and pharmaceutical analysis. All the results are found within the acceptable limits. Conclusion: The method presents a simple and reliable solution for the routine quantitative analysis of organic volatile impurities present in sumatriptan succinate API.

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