Li Zhan, Huang Xin, Jiang Zhenzhou, Xiao Yajie, Liu Chunhui, Zhang Luyong, Shu Bin, Huang Jingfeng, Li Tao, Wang Tao, Wang Feng
New Drug Screening Center, China Pharmaceutical University, Nanjing 210009, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Mar 15;864(1-2):9-14. doi: 10.1016/j.jchromb.2007.12.022. Epub 2008 Jan 4.
A sensitive and specific liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method has been developed and validated for the quantification of metacavir in rat plasma using tinidazole as an internal standard (I.S.). Following ethyl acetate extraction, the analytes were separated on a Shim-pack ODS (4.6 microm, 150 mm x 2.0 mm I.D.) column and analyzed in selected ion monitoring (SIM) mode with a positive ESI interface using the respective M+H ions, 266 for metacavir and 248 for tinidazole. The method was validated over the concentration range of 1-600 ng/mL for metacavir. Between and within-batch precisions (R.S.D.%) were all within 15% and accuracy (%) ranged from 92.2 to 105.8%. The lower limit of quantification (LLOQ) was 1 ng/mL. The extraction recovery was on average 89.8%. The validated method was used for the pharmacokinetic study of metacavir in rats.
已开发并验证了一种灵敏且特异的液相色谱 - 电喷雾电离 - 质谱(LC - ESI - MS)方法,用于以替硝唑作为内标(I.S.)定量大鼠血浆中的美他卡韦。经乙酸乙酯萃取后,分析物在Shim - pack ODS(4.6微米,150毫米×2.0毫米内径)柱上分离,并在选择离子监测(SIM)模式下使用正ESI接口,分别以M + H离子进行分析,美他卡韦为266,替硝唑为248。该方法在美他卡韦浓度范围为1 - 600 ng/mL内进行了验证。批间和批内精密度(R.S.D.%)均在15%以内,准确度(%)范围为92.2至105.8%。定量下限(LLOQ)为1 ng/mL。萃取回收率平均为89.8%。经验证后的方法用于美他卡韦在大鼠体内的药代动力学研究。