LC-MS/MS法测定Beagle犬全血中的HX0969w  

Determination of HX0969w in Beagle dogs’whole blood by LC-MS/MS

作　　者：张睿[1,2] 康仪[2] 杨俊[2] 刘进[2] 张文胜[2] 

机构地区：[1]四川大学华西药学院,四川成都610041 [2]四川大学华西医院转化神经科学中心麻醉与危重急救研究室,四川成都610041

出　　处：《华西药学杂志》2013年第4期385-387,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用LC-MS/MS法测定Beagle犬全血中异丙酚水溶性前药HX0969w的浓度。方法采用Zorbax Eclipse PlusC8色谱柱(100 mm×2.1 mm),流动相为5 mol.L-1乙酸铵水溶液-乙腈(65∶35),流速0.4 mL.min-1,进样量5μL,柱温12℃;采用三重四级杆串联质谱仪,负离子电喷雾离子源(ESI),以多反应离子模式(MRM)监测。用于定量分析的离子反应分别为m/z 343-177(HX0969w),161-89(7-羟基香豆素内标)。全血样品经含内标的甲醇溶液直接沉淀蛋白后进样。结果标准曲线的线性范围为0.05～15μg.mL-1,最低定量下限为50 ng.mL-1;日间、日内RSD均小于15%,准确度为85%～115%,符合相关规定。结论所用方法可用于HX0969w在Beagle犬体内的药动学研究。OBJECTIVE To establish a LC-MS /MS method for the determination of HX0969w in Beagle dogs’whole blood.METHODS The determination was carried on Zorbax Plus C 8（100 mm × 2.1 mm） with the mobile phase consisted of ammonium acetate（5 mol.L-1） and acetonitrile（65∶35） at a flow rate of 0.4 mL.min-1.The sample amount was 5 μL and column temperature was set at 12 ℃.Negative electrospay ionization（ESI） was used for LC-MS / MS determination.Quantification was performed in multiple reaction monitoring（MRM） mode.The ion mass spectral was m / z 343-177（HX0969w）,161-89（internal standard 7-hydroxycoumarin）.The whole blood samples were prepared by protein precipitation with methanol containing internal standard.RESULTS The calibration curve was established in the concentration range of 0.05-15 μg.mL-1.The lowest limit of quantification（LLOQ） was 50 ng.mL-1.The inter-day and intra-day accuracy were within 85%-115%.The inter-day and intra-day precision expressed as relative standard deviation（RSD） were all less than 15%.All met with the requirement.CONCLUSION The method can be used for the determination of HX0969w in Beagle dogs’whole blood and its pharmacokinetics studies.

关 键 词：前药 Beagle犬全血 HX0969w 液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]