摘要
目的建立液相色谱-串联质谱(LC-MS/MS)测定兔血浆中B07的浓度。方法血浆样品经碱化沉淀蛋白后,用甲基叔丁基醚液-液萃取,以乙腈(含0.2%乙酸)-40 mmol·L^(-1)乙酸铵(含0.2%乙酸)水溶液(80∶20)为流动相,采用Waters Symmetry C18(4.6 mm×150 mm,5μm)柱分离;采用电喷雾电离源,以多反应监测(MRM)方式进行正离子检测,用于定量分析的离子对B07为529.3→335.4,内标卡马西平为237.1→194.1。结果测定血浆中B07线性范围为0.31~310 ng·mL^(-1),r>0.99。日内和日间精密度小于15%,提取回收率均大于75%。结论该法选择性强、灵敏度高、重现性好,能够快速、准确测定兔血浆中B07浓度。
OBJECTIVE To devolop a liquid chromatographic-tandem mass spectrometric （LC-MS/MS） method for the determi- nation of B07 in rabbit plasma. METHODS Analytes were separated from plasma by a combination of alkalinized protein precipitation and liquid-liquid extraction with methyl tert-butyl ether. Chromatographic separation was performed on a Waters Symmetry C18 （4. 6 mm × 150 mm, 5 μm）column with the mobile phase consisted of acetonitrile （containing 0. 2% acetic acid ） -40 mmol·L^-1 ammonium acetate （containing 0. 2% acetic acid） in water （80：20）. A tandem mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode. Quantification was performed using muhiple reaction monitoring （MRM） of the transitions m/z 529. 3→335.4 and m/z 237.1→94. 1 for B07 and earbamazepine （internal standard）, respectively. RESULTS The method showed a good linearity in a concentration range of 0. 31 -310 ng·mL^-1 for B07 was more than 0. 99. The intra- and inter-day precision was less than 15% and the absolute recovery was above 75%. CONCLUSION This method was selec- tive and rapid, sensitive for investigating blood drug concentrations in rabbit.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2017年第12期1056-1060,共5页
Chinese Pharmaceutical Journal
基金
国家十二五重大新药创制抗艾滋病病毒新药临床评价研究技术平台建设项目资助(2012ZX09303013)
国家自然科学基金项目资助(81271834)
国家863课题"病原微生物实验室溯源和人员防护关键技术的研究"项目资助(2014AA021403)
上海市高等级生物安全病原微生物检测专业技术服务平台项目资助(15DZ2290200)
