Determination of Residual Solvents in Sulindac by Gas Chromatography
Objective:To establish a gas-phase direct injection chromatographic method for the determination of four residual solvents in sulindac API.Methods:A DB-624 capillary column(30 m×0.53 mm×3.0 μm)was used with a hydrogen flame ionization detector(FID),the carrier gas was nitrogen,and the flow rate of the column was 3.0 mL/min;the partition ratio was 15∶1;the temperature of the inlet port was 200℃;the temperature of the detector was 250℃;the temperature-rising procedure was as follows:the initial column temperature was 50℃,and then the column temperature was raised to 130℃with the rate of 20℃/min and maintained for 2 min.The initial column temperature was 50℃,then increased to 130℃at the rate of 20℃/min for 2 min,and then increased to 250℃at the rate of 50℃/min for 2 min.Results:Methanol,isopropanol,ethyl acetate and toluene could be separated efficiently under the chromatographic conditions,and the linear correlation coefficients of the respective residual solvents were 0.9999,0.9999,1.0000,and 0.9995,which were larger than 0.999,and the correlation coefficients were good.The average recoveries were 101.05%,98.90%,99.76%and 99.71%,respectively.Conclusion:The method is accurate,rapid and suitable for the detection of the four residual solvents in the API of sulindac.
gas chromatographysulinic acidresidual solventdirect injections
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