Zhao Xia, Liu Yuwang, Xu Junyu, Zhang Dan, Zhou Ying, Gu Jingkai, Cui Yimin
Department of Pharmacy, Peking University First Hospital, Beijing 100034, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Nov 1;877(29):3724-8. doi: 10.1016/j.jchromb.2009.08.025. Epub 2009 Aug 21.
A rapid, sensitive and specific liquid chromatography-tandem mass spectrometric (LC-MS/MS) method has been developed and validated for the determination of silodosin in human plasma. Silodosin and internal standard (IS) were extracted from human plasma by liquid-liquid extraction using methyl t-butyl ether and analyzed on an Agilent C(8) column with the mobile phase of acetonitrile-10 mM ammonium acetate (40:60, v/v) adjusted to pH 4.5 with acetic acid. Detection was carried out by MS/MS using TurboIonSpray (TIS) ionization and multiple reaction monitoring (MRM) in the positive-ion mode. The mass transitions monitored were m/z 496.3-->261.4 and m/z 440.4-->259.3 for silodosin and IS, respectively. The standard curve was linear in the range of 0.50-50.0 ng/ml with intra- and inter-day precision of 3.2-7.2% and 2.0-7.5%, respectively. The lower limit of quantification (LLOQ) for silodosin was 0.50 ng/ml using 500 microl plasma sample. This method was successfully applied to the pharmacokinetic study in healthy volunteers.
已开发并验证了一种快速、灵敏且特异的液相色谱-串联质谱（LC-MS/MS）方法，用于测定人血浆中的西洛多辛。采用甲基叔丁基醚通过液-液萃取从人血浆中提取西洛多辛和内标（IS），并在安捷伦C(8)柱上进行分析，流动相为乙腈-10 mM醋酸铵（40:60，v/v），用乙酸调节至pH 4.5。采用TurboIonSpray（TIS）电离和正离子模式下的多反应监测（MRM）通过MS/MS进行检测。监测的质荷比跃迁分别为西洛多辛的m/z 496.3-->261.4和内标的m/z 440.4-->259.3。标准曲线在0.50 - 50.0 ng/ml范围内呈线性，日内和日间精密度分别为3.2 - 7.2%和2.0 - 7.5%。使用500微升血浆样品时，西洛多辛的定量下限（LLOQ）为0.50 ng/ml。该方法已成功应用于健康志愿者的药代动力学研究。
