Determination of Several Residual Solvents in Dobutamine Bydrochloride by Headspace Gas Chromatography

MA Junling; PENG Yuhui

doi:10.3969/j.issn.2096-305X.2025.02.004

Abstract：Objective To establish a headspace gas chromatography method that can simultaneously determine five residual solvents of dobutamine hydrochloride for the quality control of dobutamine hydrochloride apis,and verify the analytical method for detection of residual solvents of dobutamine hydrochloride to ensure that the residual solvents of the apis can meet the internal quality standards.Methods Headspace-Gas Chromatography was performed in DB-624 quartz capillary column(30 m×0.32 mm,1.8 μm,6.0％cyanopropyl phenyl,94.0％dimethylsiloxane).The detector was a hydrogen flame ionization detector(FID)with N-methylpyrrolidone∶water 95∶5 as solvent.Programmed temperature rise:The initial temperature is 45 ℃ for 5 min,and the temperature rises to 240 ℃ at the rate of 10 ℃/min for 3 min;running time 27.5 min.Results The mass concentrations of ethanol,acetone,dichloromethane,ethyl acetate and cyclohexane in the range of 6.512-1007.760,1.606-1024.440,6.075-121.500,1.757-1013.100,0.271-200.406 μg/mL were linearly correlated with the peak area(r ≥ 0.9997,n=7);the limits of quantification were 6.512,1.606,6.075,1.757,0.271 μg/mL,and the limits of detection were 1.954,0.482,1.823,0.527,0.081 μg/mL,respectively.RSD of repeatability test was less than 2.0％(n=6).The recoveries of ethanol,acetone,dichloromethane,ethyl acetate and cyclohexane were 103.5％-107.1％,106.8％-108.3％,109.2％-110.9％,111.6％-113.4％and 111.6％-113.4％at 50.0％,100.0％and 150.0％,respectively.RSDS were 1.3％,0.5％,0.6％,0.5％,and 0.5％,respectively(n=9).None of the 5 residual solvents were detected in the samples.Conclusion The method is easy to operate,accurate,reliable and sensitive,and can be used for the determination of residual organic solvents of ethanol,acetone,dichloromethane,ethyl acetate and cyclohexane in dobutamine hydrochloride raw materials.