摘要
目的建立小鼠血浆及脑组织中马钱子碱浓度的UPLC-MS/MS测定方法 ,用于小鼠马钱子碱药动学研究。方法色谱柱为Acquity UPLC BEHC18柱(2.1mm×50mm,1.7μm)。流动相为水(含0.1%甲酸)-甲醇(75:25,v/v),流速0.25mL.min-1,柱温40℃。吗氯贝胺为内标,采用ESI+模式,多重反应选择离子检测,马钱子碱m/z395→324,吗氯贝胺m/z269→182。样品处理采用液液萃取。结果马钱子碱在小鼠血浆中线性范围为5.016～5016ng.mL-1,脑组织中线性范围为3.009～725.4ng.g-1,日内精密度(RSD)均<8.5%,日间精密度(RSD)均<11.2%,方法回收率范围血浆中为91.7%～112.9%,脑组织中为95.6%～107.2%。结论本方法简单、灵敏、准确,适用于小鼠体内马钱子碱浓度测定及药动力学研究。
Objective To develop an ultra-performance liquid chromatography tandem mass spectrometry for the determination of brucine in mice plasma and brain.Methods Acquity UPLC BEH C18 column（2.1 mm×50 mm,1.7 μm） was used with methanol-0.1% formic acid（25：75,v/v）as the mobile phase at 0.25 mL·min-1.The column temperature was 40℃.UPLC-ESI＋-MS/MS was performed in the multiple reaction monitoring （MRM） mode using target ions at m/z 395→324 （brucine）and m/z 269→182（IS）.The samples were extracted from mice plasma and brain using liquid-liquid extraction.Results The calibration curve of brucine was linear over 5.016-5 016 ng·mL-1 in the plasma,3.009-725.4 ng·g-1 in the brain.The methodology recovery was 91.7%-112.9% and 95.6%-107.2% in the plasma and the brain respectively.Inter-day and intra-day RSDs were all less than 15%.Conclusion The method is simple,sensitive and accurate for the study of brucine in mice.
出处
《中南药学》
CAS
2010年第5期321-325,共5页
Central South Pharmacy
基金
湖南省中医药科研计划项目课题(No.2008086)
关键词
马钱子碱
超高效液相色谱-串联质谱
brucine
ultra-performance liquid chromatography tandem mass spectrometry
