Determination of Residual Solvents in Paeoniflorin-6'-O-benzene Sulfonate by Headspace Capillary GC
Objective:To establish a GC method for the determination of residual solvents in paeoniflorin-6'-O-benzene sulfonate.Methods:The residual solvents in paeoniflorin-6'-O-benzene sulfonate were separated and detected by HP-INNOWAX capillary column(0.53 mm×30 m,1 μm)with FID detector.The carried gas was nitrogen,and the gas flow rate was 5 mL/min.The column temperature was programmed.The inlet temperature was 120℃and FID detector temperature was set at 260℃.Headspace conditions were as follows:the time and the temperature of balance for the sample were 80℃and 30 min;the temperature of quantitative loop and transfer lines was 95℃and 90℃,respectively.Results:The 6 residual solvents tested were completely separated and the linear relationship was good.The LOQ of methanol,ethanol,acetone,chloroform,ethyl acetate and dimethyl carbonate were 10.0 mg/kg,5.0 mg/kg,1.0 mg/kg,1.5 mg/kg,1.0 mg/kg and 5.0 mg/kg,and the LOD of them were 3.0 mg/kg,1.5 mg/kg,0.3 mg/kg,0.45 mg/kg,0.3 mg/kg and 1.5 mg/kg,respectively.The RSD of recovery,precision,repeatability and stability were all less than 10%.Conclusion:In general,this method can be used to determine the residual solvents in paeoniflorin-6'-O-benzene sulfonate,and provides the material basis for the quality control of paeoniflorin-6'-O-benzene sulfonate.
NETL
NSTL
万方数据
