顶空-气相色谱法测定芍药苷-6'-O-苯磺酸酯中的残留溶剂

Determination of Residual Solvents in Paeoniflorin-6'-O-benzene Sulfonate by Headspace Capillary GC

目的:建立顶空-气相色谱法测定芍药苷-6’-O-苯磺酸酯中的6种残留溶剂的测定方法。方法:采用顶空-气相色谱法,HP-INNOWAX(0.530 mm×30 m,1μm)石英毛细管柱,氢火焰离子化检测器,载气为氮气,流速5 mL/min;柱温为程序升温,进样口温度为120℃,检测器温度260℃。顶空进样条件:顶空平衡时间为30 min,平衡温度80℃,定量环温度95℃,传输线温度90℃。结果:测定的6种有机溶剂完全分离,在相应浓度范围内线性关系良好。甲醇、乙醇、丙酮、三氯甲烷、乙酸乙酯和碳酸二甲酯的定量限分别是10.0 mg/kg,5.0 mg/kg,1.0 mg/kg,1.5 mg/kg,1.0 mg/kg和5.0 mg/kg,检测限分别是3.0 mg/kg,1.5 mg/kg,0.3 mg/kg,0.45 mg/kg,0.3 mg/kg和1.5 mg/kg。加标回收率、精密度、重复性和耐用性的RSD均小于10%。结论:本方法可以较好地用于测定芍药苷-6’-O-苯磺酸酯中的残留溶剂,对芍药苷-6’-O-苯磺酸酯的质量控制提供了科学依据。

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,1μm)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.