液相色谱-串联质谱法测定人血浆中阿米卡星、地塞米松和利巴韦林的浓度  

Quantitative Determination of Amikacin Dexamethasone and Ribavirin in Human Plasma by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张聪[1] 梅清华[1] 卢慧勤[1] 林壮民[1] 梁金成[1] 

机构地区：[1]广东省第二人民医院药学部,广州510317

出　　处：《中国药学杂志》2016年第11期920-924,共5页Chinese Pharmaceutical Journal

基　　金：广东省科学技术厅资助项目(2013B090600144)

摘　　要：目的建立高效液相色谱-串联质谱法同时测定人血浆中阿米卡星、地塞米松和利巴韦林浓度的分析方法。方法血浆样品经甲醇沉淀蛋白,以卡那霉素为内标,采用Inertsil HILIC柱(2.1 mm×150 mm,3.5μm)分离,流动相组成包括乙腈(含体积分数0.1%甲酸)和水(含体积分数0.1%甲酸),梯度洗脱,流速0.4 m L·min^(-1)。通过电喷雾离子化,采用正离子检测。结果阿米卡星、地塞米松和利巴韦林的线性范围分别为1.038~1 038,1.063~1 063,1.029~1 029 ng·m L^(-1),相关系数(r≥0.99),定量下限分别为1.038,1.063,1.029 ng·m L^(-1)。日内及日间精密度小于13.7%,准确度的相对误差(RE)在-9.2%~10.9%。结论该方法高效、灵敏、特异性强,准确度、精密度好,适用于阿米卡星、地塞米松和利巴韦林药物动力学分析实验。OBJECTIVE To develop a high performance liquid chromatography-tandem mass spectrometry( HPLC-MS / MS)method for determination of amikacin,dexamethasone,and ribavirin in human plasma. METHODS With kanamycin as internal standard( IS),samples involve a one-step extraction with methanol of 0. 2 m L plasma. The analysis was carried out on the Inertsil HILIC( 2. 1 mm × 150 mm,3. 5 μm) column with gradient elution at a flow rate of 0. 4 m L·min^(-1). The mobile phase was acetonitrile( containing 0. 1% formic acid) and 0. 1% formic acid. The determination was performed on a triple quadrupole tandem mass spectrometer by multiple reactions monitoring( MRM) mode via electrospray ionization( ESI) source. RESULTS The standard curves were linear( r≥ 0. 999) over the concentration range of 1. 038- 1 038 ng·m L^(-1)( amikacin),1.063- 1063 ng·m L^(-1)( dexamethasone),and 1. 029- 1 029 ng · mL^(-1)( ribavirin) with the lower limit of quantification( LLOQ) of 1. 038,1. 063,1. 029 ng·m L^(-1). The intra- and inter-day precision( RSD) value was below 13. 7 % and accuracy( relative error) was ranged from-9.2 % to 10. 9 % at all three quality control( QC) level. CONCLUSION The method for determination of amikacin,dexamethasone,and ribavirin in human plasma is rapid sensitive and accurate,as well as suitable to evaluate the and forensic toxicological analysis.

关 键 词：阿米卡星 地塞米松 利巴韦林 高效液相色谱-串联质谱法 药动学 

分 类 号：R969.1[医药卫生—药理学]