顶空毛细管气相色谱法测定盐酸右美托咪定中残留溶剂含量  

Quantification of Residual Organic Solvents in Dexmedetomidine Hydrochloride by Headspace Capillary Gas Chromatography

作　　者：杨园 谷亦平 YANG Yuan;GU Yiping(Wuhan Pharmaceutical Medical Device Inspection Institute,Wuhan 430073,China;School of Public Health,Guilin Medical College,Guilin 541199,China)

机构地区：[1]武汉药品医疗器械检验所,武汉430073 [2]桂林医学院公共卫生学院,桂林541199

出　　处：《医药导报》2021年第7期927-930,共4页Herald of Medicine

基　　金：湖北省食品药品监督管理局2016-2017年度科研项目(201601017)。

摘　　要：目的建立顶空毛细管气相色谱法测定盐酸右美托咪定中11种残留溶剂含量。方法色谱柱为Agilent DB-624毛细管柱,采用程序升温,检测器为氢火焰离子化检测器,检测器温度250℃,以水为溶剂,外标法计算残留溶剂的含量。结果甲醇、乙醇、乙醚、丙酮、异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、环己烷、二氧六环、甲苯色谱峰均能得到有效分离;所测残留溶剂在各自浓度范围内呈良好的线性关系(r=0.9991~0.9999);平均回收率97.2%~100.3%(RSD=0.6%~2.1%);定量限分别为1.13,1.05,0.09,0.39,0.78,0.43,0.46,0.48,0.68,8.00,0.27μg·mL^(-1)。结论该方法简单、可靠、准确,可用于盐酸右美托咪定原料中有机溶剂残留量的检测。Objective To establish a new method of headspace capillary gas chromatography for determination of eleven residual organic solvents in raw material drug of dexmedetomidine hydrochloride.Methods The separation was achieved on Agilent DB-624 capillary column using temperature programming.Flame ionization detector(FID)was chosen as the detector with the temperature set at 250℃and water was used as the solvent.The analysis of residual solvents was evaluated by external standard method.Results Methanol,ethanol,diethyl ether,acetone,isopropyl alcohol,dichloromethane,acetidin,tetrahydrofuran,cyclohexane,dioxane,and toluene were completely separated.Calibration curves for all components were linear within the studied ranges(r=0.9991-0.9999).Average recoveries were in the range of 97.2%-100.3%with RSD 0.6%-2.1%.The limits of quantification were 1.13,1.05,0.09,0.39,0.78,0.43,0.46,0.48,0.68,8.00,and 0.27μg·mL^(-1),respectively.Conclusion The method is simple,reliable and accurate;and it can be used for the determination of residual organic solvents in dexmedetomidine hydrochloride.

关 键 词：盐酸右美托咪定 残留溶剂 顶空毛细管气相色谱法 含量测定 

分 类 号：R971.2[医药卫生—药品] R927.1[医药卫生—药学]