School of Pharmacy, Sungkyunkwan University, Suwon 440-746, Republic of Korea.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Nov 15;909:65-9. doi: 10.1016/j.jchromb.2012.10.012. Epub 2012 Oct 13.
Tamsulosin, a selective α₁-adrenoceptor antagonist, is used for the treatment of benign prostatic hyperplasia (BPH). We developed and validated a rapid, sensitive, and simplified liquid chromatography analytical method utilizing tandem mass spectrometry (LC-MS/MS) for the determination of tamsulosin in human plasma. After liquid-liquid extraction with methyl t-butyl ether, chromatographic separation of tamsulosin was achieved using a reversed-phase Luna C₁₈ column (2.0 mm × 50 mm, 5 μm particles) with a mobile phase of 10 mM ammonium formate buffer (pH 3.5)-methanol (25:75, v/v) and quantified by MS/MS detection in ESI positive ion mode. The flow rate of the mobile phase was 200 μL/min and the retention times of tamsulosin and the internal standard (IS, diphenhydramine) were 0.8 and 0.9 min, respectively. The calibration curves were linear over a range of 0.01-20 ng/mL (r>0.999). The lower limit of quantification using 500 μL of human plasma was 0.01 ng/mL. The mean accuracy and precision for intra- and inter-day validation of tamsulosin were both within acceptable limits. The present LC-MS/MS method showed improved sensitivity for quantification of tamsulosin in human plasma compared with previously described analytical methods. The validated method was successfully applied to a pharmacokinetic study in humans.
坦索罗辛是一种选择性α₁-肾上腺素受体拮抗剂,用于治疗良性前列腺增生(BPH)。我们开发并验证了一种快速、灵敏、简化的液相色谱分析方法,利用串联质谱(LC-MS/MS)测定人血浆中的坦索罗辛。经甲基叔丁基醚液液萃取后,采用反相 Luna C₁₈柱(2.0mm×50mm,5μm 颗粒),以 10mM 甲酸铵缓冲液(pH3.5)-甲醇(25:75,v/v)为流动相进行色谱分离,在电喷雾正离子模式下进行 MS/MS 检测定量。流动相的流速为 200μL/min,坦索罗辛和内标(IS,苯海拉明)的保留时间分别为 0.8 和 0.9min。校准曲线在 0.01-20ng/mL 范围内呈线性(r>0.999)。使用 500μL 人血浆的定量下限为 0.01ng/mL。坦索罗辛日内和日间验证的平均准确度和精密度均在可接受范围内。与以前描述的分析方法相比,本 LC-MS/MS 方法显示出提高的检测灵敏度。该验证方法已成功应用于人体药代动力学研究。