摘要
建立了LC-MS法测定人血浆中的螺内酯(1)及其代谢物坎利酮(2)。以劳拉西泮(3)为内标,乙酸乙酯-二氯甲烷(4∶1)为提取溶剂,采用C18柱,流动相为甲醇-水(65∶35)。采用大气压化学离子化源,选择性监测质荷比(m/z)为341.2(1和2)和321.0(3)的离子峰。碎片电压分别为130V(1和2)和140V(3)。结果显示1和2均在2～300ng/ml浓度范围内线性关系良好,定量限为2.0ng/ml,日内、日间RSD均小于10%。
A LC-MS method was established for the determination of spironolactone （1） and its metabolite canrenone （2） in human plasma with lorazepam （3） as the internal standard. 1 and 2 in plasma were extracted with ethyl acetate-dichlormethane （4： 1）. A C18 column was used with mobile phase of methanol-water （65：35）. The compounds were ionized in the atmospheric pressure chemical ionization （APCI） and detected in the selected ion monitoring （SIM） mode （m/z 341.2 for 1 and 2, m/z 321.0 for 3）, and the fragment voltage of 130V for 1 and 2, 140V for 3. The calibration curve was linear for 1 and 2 in the concentration range of 2 - 300ng/ml with the LLOQ of 2.0ng/ml. The intra- and inter-day RSDs were less than 10 %.
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2008年第11期842-845,共4页
Chinese Journal of Pharmaceuticals
