顶空-气相色谱法测定丹酚酸A提取物的溶剂残留量  

Determination of Solvent Residue in Salvianolic Acid A by Headspace Gas Chromatography

作　　者：邱小燕 王章伟 王振 刘芳芳 刘地发 钟仁清 QIU Xiaoyan;WANG Zhangwei;WANG Zhen;LIU Fangfang;LIU Difa;ZHONG Renqing(Jiangxi Qingfeng Pharmaceutical Co.,Ltd.,Ganzhou 341000,China;Jiangxi Kerui Pharmaceutical Co.,Ltd.,Ganzhou 341000,China)

机构地区：[1]江西青峰药业有限公司,江西赣州341000 [2]江西科睿药业有限公司,江西赣州341000

出　　处：《山东化工》2024年第23期155-158,161,共5页Shandong Chemical Industry

基　　金：江西省科技创新平台组建(20194AFD45002);江西省重点研发计划项目(20203BBG73065)。

摘　　要：目的:建立顶空-气相色谱法测定丹酚酸A提取物中甲基叔丁基醚、环己烷、乙醇3种溶剂残留的分析方法,提高提取物质量控制水平。方法:采用HP-INNOWAX聚乙二醇为固定相的毛细管柱(30 m×0.32 mm×0.5μm)。供试品顶空进样,平衡温度90℃,平衡时间30 min,分流比20∶1(体积比),氢火焰离子化检测器(FID)进行分析。结果:3种残留溶剂分离效果较好,在各自限度浓度的80%~120%范围内线性、精密度、准确度良好;回收率均在80%~120%,相对标准偏差≤10%(n=9)。3批中试样品中溶剂残留均符合中国药典要求。结论:方法经验证均符合要求,且该方法操作方便,结果稳定可靠,可用于丹酚酸A提取物中残留溶剂的检测。Objective:Establish a method for determining methyl tert-butyl ether,cyclohexane,ethanol solvent residues in salvianolic acid A(SAA)and improve the quality control level.Methods:The capillary column using HP-INNOWAX polyethylene glycol as the stationary phase.Test sample was injected through headspace injection.The equilibrium temperature of the headspace was 90℃,and equilibrium time was 30 minutes.Split ratio was 20∶1(volume ratio).The detector was hydrogen flame ionization detector(FID).Results:The separation effect of three residual solvents were very well,with good linearity,precision,and accuracy between 80% and 120% of their respective limit concentrations.The recovery rates were all within the range of 80% to 120% and RSD≤10%(n=9).The solvent residues in the three batches of pilot samples were all meet the requirements of the Chinese Pharmacopoeia.Conclusion:The method has been validated to meet the requirements and the results were stable and reliable.It can be used for the detection of residual solvents in salvianolic acid A.

关 键 词：丹酚酸A 溶剂残留量 顶空-气相色谱法 质量控制 安全风险 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.71[化学工程—制药化工]