盐酸艾司洛尔残留溶剂测定方法优化  

Optimization of determination method for residualsolvents of esmolol hydrochloride

作　　者：陈思明[1] 翁贤坤 孙海芸 罗宗玉 CHEN Siming;WENG Xiankun;SUN Haiyun;LUO Zongyu(Wuzhishan Branch of Hainan Provincial Food and Drug Inspection Institute,Wuzhishan 572299,China;Hainan Beite Pharmaceutical Co.,Ltd,Haikou 572000,China)

机构地区：[1]海南省食品药品检验所五指山分所,海南五指山572299 [2]海南倍特药业有限公司,海口572000

出　　处：《中国药品标准》2024年第2期154-158,共5页Drug Standards of China

摘　　要：目的:优化盐酸艾司洛尔残留溶剂检测方法,以便于内部质量控制。方法:使用气相色谱顶空进样方式,选择合适的顶空平衡温度和时间,降低样品对仪器的污染,优化溶剂比例,降低基质效应,调整了载气流速和分流比,采用极性毛细管柱程序升温的方法,延长了高温段保持时间等,并进行方法学验证。结果:乙醚、乙酸乙酯、甲醇、甲苯均能得到有效分离,精密度良好,峰面积和质量浓度均呈很好的线性关系,分别考察样品加标50%、100%、150%3个浓度的准确度,平均回收率均能在94.8%~105.6%。结论:该方法准确,灵敏度高,克服了《中国药典》方法的缺陷,可用于盐酸艾司洛尔残留溶剂检测。Objective:To optimize the detection method for residual solvents of esmolol hydrochloride for control of internal quality.Methods:Gas chromatography headspace injection method was adopted by selecting appropriate headspace equilibrium temperature and time in order to reduce sample contamination of the instrument,optimizing solvent ratio for reducing matrix effect and adjusting carrier gas flow rate and split ratio.Polar capillary column programmed temperature rise method was used with high temperature holding time,etc.,and methodological validation was conducted.Results:Ether,ethyl acetate,methanol,and toluene could all be effectively separated with good precision,and there were good linear relationships between peak areas and mass concentrations.The accuracy of sample spiking at 50%,100%,and 150%concentrations was investigated,and the average recovery rates could all reach ranges of 94.8%-105.6%.Conclusion:This method is accurate,highly sensitive,and overcomes the shortcomings of the Chinese Pharmacopoeia methods.It can be used for the detection of residual solvents in esmolol hydrochloride.

关 键 词：盐酸艾司洛尔 残留溶剂 顶空进样 方法优化 毛细管气相色谱 方法学验证 

分 类 号：R921.2[医药卫生—药学]