UPLC-MS/MS法测定比格犬血浆中双氯芬酸钠的浓度  

UPLC-MS/MS determination of the diclofenac sodium(DS) in dog plasma

作　　者：向志雄[1] 刘文丽[1] 

机构地区：[1]上海医药集团股份有限公司中央研究院,上海201203

出　　处：《上海医药》2015年第5期74-77,共4页Shanghai Medical & Pharmaceutical Journal

摘　　要：目的 ：建立灵敏的超高效液相色谱-质谱联用法测定比格犬血浆中的双氯芬酸钠的浓度。方法 ：选用BEH C18（2.1 mm×100 mm,1.7 mm）色谱柱,以乙腈-醋酸铵（2 mmol·L-1）-甲酸（70∶30∶0.1,v/v/v）为流动相,采用等度洗脱进行分离,样品采用含0.1%甲酸的乙腈进行蛋白沉淀后进样,通过电喷雾电离源,以多重反应监测（MRM）方式进行负离子检测,用于定量分析的离子对为m/z（293.9＋293.9＋296.1）→（249.9＋213.7＋251.8）（双氯芬酸）和m/z283.0→239.0（内标,大黄酸）测定双氯芬酸钠。结果 ：双氯芬酸钠的线性范围为：1.0~3 000.0 ng·ml-1;定量下限可达1.0 ng·ml-1;日内、日间精密度（RSD）均小于15%。结论 ：本方法同时选择3个碎片离子作为双氯芬酸钠定量产物离子,明显的改进了分析方法的灵敏度,血浆用量少,适用于比格犬血浆样品中双氯芬酸钠的测定和药物动力学研究。Objective： To develop a UPLC-MS/MS method for determination of diclofenac sodium（DS） in dog plasma. Methods： DS and internal standard were extracted from plasma by acetonitrile containing 0.1% formic acid and separated on a column BEH C18（2.1 mm×100 mm, 1.7 mm）using acetonitrile-ammonium acetate（2 mmol·L-1）-formic acid（0.1%）（70 ∶ 30 ∶ 0.1, v/v/v） as a mobile phase. A tandem mass spectrometer equipped with electrospray ionization source was adopted as a detector. Multiple reaction monitoring（MRM） transitions of m/z（293.9＋293.9＋296.1） →（249.9＋213.7＋251.8）, m/z283.0→239.0 were measured in negative mode for DS and internal standard rhein, respectively. Results： The calibration curve for DS was linear over the range of 1.0~3 000.0 ng·ml-1 and the lower limit of quantification was 1.0 ng·ml-1 with the relative standard deviation of intra-day and inter-day over the entire concentration range less than 15%. Conclusion： This method is sensitive and suitable for pharmacokinetic study of DS in dog subjects.

关 键 词：超高效液相色谱-质谱联用法 双氯芬酸钠 比格犬血浆样品检测 血药浓度 

分 类 号：R965[医药卫生—药理学] O657.63[医药卫生—药学]