HPLC-MS法测定血浆中左旋黄皮酰胺的浓度  

Quantitation of(-)Clausenamide in Plasma with LC-MS

作　　者：钱文[1] 宋敏[2] 杭太俊[2] 张正行[2] 

机构地区：[1]江苏省药品检验所,南京210008 [2]中国药科大学药物分析室,南京210009

出　　处：《药物分析杂志》2005年第4期446-448,共3页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立测定血浆中左旋黄皮酰胺浓度的 LC-MS 方法。方法:血浆样品经醋酸乙酯提取处理后,以2%冰醋酸-甲醇(45∶55)为流动相,在1.0 mL·min^(-1)的流速下,用 Shimadzu ODS 色谱柱(150mm×4.6mm,5μm)分离,样品经电喷雾离子化后,通过 HP 1100 HPLC-MS 质谱仪液相色谱串联质谱法,以格列吡嗪为内标测定左旋黄皮酰胺的浓度。结果:血浆中左旋黄皮酰胺的线性范围为0.01-10μg·mL^(-1),最低定量浓度为10ng·mL^(-1),准确度在80%-90%之间,日内、日间精密度(RSD)在±10%之内。结论:该方法高效、准确,可用于左旋黄皮酰胺在体内的药代动力学研究及血浆中左旋黄皮酰胺的含量测定以控制质量。Objective:To establish an LC-MS method to determine (-) clausenamide in plasma.Method:Plas- ma samples were extracted by ethyl acetate,then separated on a Shimadzu ODS (150 mm×4.6 mm,5 μm)colume with 2% acetic acid glacial-methanol(45:55)as mobile phase,at a flow rate of 1.0 mL·min^(-1).Eleetrospray ion- ization source(ESI) was applied and operated in positive ion mode.(-)Clausenamide was quantified by HP 1100 HPLC-MS using glipiside as the internal reference.Results:The linear calibrate curves were obtained over the concentration range of 0.01-10 μg·mL^(-1) and the lower limit of quantitation was 10 ng·mL^(-1).Accuracy was within 80%-90%,and inter-and intra-day precision (RSD) were within±10%.Conliusion:The method proved to be effective and accurate,and can be applied to the pharmacokinetic study and quanlity control of(-) clausenamide.

关 键 词：左旋黄皮酰胺 HPLC MS法 液相色谱串联质谱法 药代动力学研究 ODS色谱柱 电喷雾离子化 醋酸乙酯 血浆样品 格列吡嗪 线性范围 控制质量 含量测定 流动相 冰醋酸 质谱仪 量浓度 准确度 精密度 

分 类 号：R969.1[医药卫生—药理学] R286.0[医药卫生—药学]