气相色谱法测定人血白蛋白中乙醇残留量  

Determination of residual ethanol in the human albumin

作　　者：陈宇堃[1] 刘丛丛[1] 梁蔚阳[1] CHEN Yukun;LIU Congcong;LIANG Weiyang(Guangdong Institute for Drug Control,NMPA Key Laboratory for Quality Control of Blood Products,Guangdong Drug Administration Key Laboratory of Quality Control and Research of Blood Products,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,国家药品监督管理局血液制品质量控制重点实验室,广东省药品监督管理局血液制品质量控制研究重点实验室,广州510663

出　　处：《中国药品标准》2022年第3期302-309,共8页Drug Standards of China

基　　金：广东省医学科学技术研究基金项目(B2021371);广东省药品监督管理局科技创新项目(2021ZDZ02)。

摘　　要：目的:建立气相色谱法测定人血白蛋白中乙醇残留量。方法:采用DB-624毛细管色谱柱(30 m×0.32 mm×1.8μm);氢火焰离子化检测器(FID);进样口温度为200℃,检测器温度为250℃;载气为氮气,载气流速为2.0 mL·min^(-1);采用程序升温法:起始温度为40℃,保持8 min,以50℃·min^(-1)速度升温至200℃,保持5 min。进样方式为顶空进样,顶空平衡温度为80℃,平衡时间为30 min。结果:乙醇在1.0056~377.0975μg·mL^(-1)范围内与峰面积线性关系良好(r为0.9998,n=9);精密度的RSD为2.5%,重复性的RSD为1.5%;平均加样回收率为100.2%(n=9,RSD为3.4%)。定量限为1.0056μg·mL^(-1),检出限为0.3352μg·mL^(-1)。测定人血白蛋白原液59批和成品78批,均低于250μg·mL^(-1)。结论:该方法操作简单、结果准确,灵敏度高,专属性强,可用于人血白蛋白中乙醇残留量测定。Objective:To establish a method for the determination of residual ethanol in human albumin.Methods:The determination was performed in DB-624 capillary chromatography column(30 m×0.32 mm×1.8μm).FID detector was used,the inlet temperature was 200℃and the detector temperature was 250℃.The carrier gas was nitrogen and the flow rate of carrier gas was 2.0 mL·min^(-1).The column temperature program was set as:remaining the starting temperature of 40℃for 8 min,then increasing to 200℃at the rate of 50℃·min^(-1) and remaining 200℃for 5 min.The headspace injection was used,the headspace equilibrium temperature was 80℃,and the equilibration time was 30 min.Results:The linear range of ethanol fell into 1.0056-377.0975μg·mL^(-1) with r=0.9998(n=9).The RSD of precision was 2.5%,and the RSD of repeatability was 1.5%.The average recovery was 100.2%(n=9,RSD=3.4%).The limit of quantitation was 1.0056μg·mL^(-1),and the limit of detection was 0.3352μg·mL^(-1).All the test results of 59 batches of the stock solution of human albumin stock solution and 78 batches of finished products were less than 250μg·mL^(-1).Conclusion:The established method is simple and accurate,and has the high sensitivity and good specificity.It can be applicable to the determination of residual ethanol in human albumin.

关 键 词：人血白蛋白 乙醇 残留溶剂 气相色谱法 

分 类 号：R921.2[医药卫生—药学]