LC-MS/MS法测定比格犬血浆中伊曲康唑浓度的方法建立及不确定度评定  

Establishment of Method and Uncertainty Evaluation for Determination of Itraconazole in Beagle Plasma by LC-MS/MS

作　　者：刘艳芳 张晓 蔡朝红 LIU Yan-fang;ZHANG Xiao;CAI Chao-hong(General Hospital of Northern Theater Command,Shenyang 110840,China;Hebei Eye Hospital,Xingtai 054001,China)

机构地区：[1]北部战区总医院,辽宁沈阳110840 [2]河北省眼科医院,河北邢台054001

出　　处：《解放军药学学报》2024年第5期438-442,共5页Pharmaceutical Journal of Chinese People's Liberation Army

基　　金：邢台市重点研发计划项目,No.2023ZZ056。

摘　　要：目的建立测定比格犬血浆中伊曲康唑浓度的液相色谱串联质谱法,并进行不确定度评定。方法采用Waters Xevo TQD液质联用仪,BEH C_(18)色谱柱;以0.2%甲酸水-0.2%甲酸乙腈(20∶80)为流动相,甲基叔丁基醚为萃取剂建立检测方法;依据《中国药典》(2020年版)对新建定量分析方法进行方法验证,依据国家计量检定相关规程对方法不确定度进行评定。结果方法专属性、线性等各项均符合《中国药典》要求,方法不确定度主要由线性拟合引入。结论该法准确可靠,可用于比格犬血浆中伊曲康唑浓度的测定,本研究按试验流程进行不确定度分量量化,此法简单、准确适合生物分析方法的不确定度评定。Objective To establish a method for the determination of Itraconazole in beagle plasma by LC-MS/MS and evaluate its uncertainty.Methods Waters Xevo TQD high-performance liquid chromatography tandem mass spectrometer with a C18 column was used.The mobile phase consisted of 0.2%formic acid water and 0.2%formic acid acetonitrile(20∶80)with methyltert butylether as the extractant.The applicability of this method was verified according to the Chinese pharmacopoeia while its uncertainty was evaluated according to the related national regulations concerning metrological verification.Results The specificity and linearity of the method met the requirements of Pharmacopoeia.The uncertainty was mostly introduced by linear fitting.Conclusion This method is accurate and reliable,which can be used for the determination of Itraconazole concentrations in beagle plasma.

关 键 词：伊曲康唑 液相色谱串联质谱分析 不确定度 

分 类 号：R917[医药卫生—药物分析学]