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
白柏 1叶文才 2刘菊妍 3许文东 4许一靖4
作者信息
- 1. 暨南大学,广东 广州 510000;中药制药过程技术与新药创制国家工程研究中心,广州白云山汉方现代药业有限公司,广东 广州 510240
- 2. 暨南大学,广东 广州 510000
- 3. 广州医药集团有限公司,广东 广州 510006
- 4. 中药制药过程技术与新药创制国家工程研究中心,广州白云山汉方现代药业有限公司,广东 广州 510240
- 折叠
摘要
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,1 μm)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.
Abstract
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.
关键词
芍药苷-6'-O-苯磺酸酯/气相色谱/残留溶剂/顶空进样Key words
paeoniflorin-6'-O-benzene sulfonate/gas chromatography/residual solvents/headspace injection引用本文复制引用
出版年
2024
NETL
NSTL
万方数据