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目的建立同时测定人血浆中卢帕他定及其主要活性代谢产物地洛他定浓度的LC-MS/MS法。方法以艾司唑仑为内标,血浆样品经环己烷-乙醚(50∶50,V/V)提取后,以甲醇-乙酸铵溶液(5 mmol/L,p H=2.2)(70∶30,V/V)为流动相,采用Shimadzu ODS色谱柱(150 mm×2.0 mm,5μm)分离,电喷雾离子化-正离子选择性检测方式,检测离子为m/z:416.1→309.0(卢帕他定),311.2→295.0(地洛他定),295.0→267.1(内标艾司唑仑)。结果卢帕他定浓度在0.1 ng/ml~100.0 ng/ml、地洛他定浓度在0.1 ng/ml~50.0 ng/ml线性关系良好(r>0.99),最低检测限浓度均达0.05 ng/ml,高、中、低3种浓度的平均提取回收率均>70%,批内、批间精密度良好(RSD<15%)。结论该方法样品前处理简便、灵敏度高、精密度好、线性范围宽,为卢帕他定大批量生物样本的分析提供了新的选择。
Objective To establish a LC-MS / MS method for the simultaneous determination of loratadine and its major active metabolite of loratadine in human plasma. Methods Estazolam was used as an internal standard. The plasma samples were extracted with cyclohexane-ether (50:50, V / V) and eluted with methanol-ammonium acetate solution (5 mmol / L, p H = 2.2) 30, V / V) as the mobile phase. The separation was performed on a Shimadzu ODS column (150 mm × 2.0 mm, 5 μm) using electrospray ionization-positive ion selective detection. The detection ion was m / z: 416.1 → 309.0 Paclitaxel), 311.2 → 295.0 (Dextauidine), 295.0 → 267.1 (Estazolam, internal standard). Results The linearity of ropassatine between 0.1 ng / ml and 100.0 ng / ml and that of loratadine between 0.1 ng / ml and 50.0 ng / ml was good (r> 0.99), and the lowest detection limit was 0.05 ng / ml. The average extraction recoveries of high, medium and low concentrations were> 70%. The intra-assay and inter-assay precision were good (RSD <15%). Conclusions The method is simple, sensitive, accurate, and linear. It provides a new choice for the analysis of large batch biological samples of rupatadine.