In order to establish the quality control system of retigabine active substances,a headspace gas chromatographic method was established and validated for the determination of residual solvents of ethanol,hexane,tetrahydrofuran and triethylamine in retigabine active substances,by using FID as the detector and N,N-dimethylformamide as sample solvent.The detection of four residual solvents was performed on a DB-624 capillary column with vial equilibration temperature of 110 ℃ and equilibration time of 15 min.The limits of detection(LOD) for ethanol,hexane,tetrahydrofuran and triethylamine were 0.007 5%,0.000 48%,0.002 4% and 0.01%,respectively.The relative standard deviations(RSDs) of peak areas were below 2.1%.The average recoveries were in the range of 100%-102%, and the correlation coefficients were above 0.995.The result indicated that the method showed the advantages of high sensitivity,good accurancy and linearity.The established method was applied in the quality control of three batches of retigabine,and only ethanol and hexane were checked out with the highest residual level of 0.149% and 0.022%,respectively,which did not exceed the limited quantity.
关键词
瑞替加滨顶空气相色谱法残留溶剂乙醇正己烷四氢呋喃三乙胺
Keywords
retigabineheadspace gas chromatographic methodresidual solventsethanolhexanetetrahydrofurantriethylamine
Determination of Earthy-musty Odorants in Tap Water by Gas Chromatography-Mass Spectrometry with Dispersion Solid-phase
RP-HPLC Determination of Ester and Organic Acids in the Oxidative Products of Tetrahydrofuran with Molecular Oxygen
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Key Laboratory of Oceanic and Polar Fisheries,Ministry of Agriculture and Rural Affairs,East China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences
Qingdao Municipal Center for Disease Control and Prevention
Key Laboratory of East China Sea Fishery Resources Exploitation,Ministry of Agriculture and Rural Affairs,East China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences