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采用液相色谱/串联质谱法测定人血浆中的坦索罗辛及其在药代动力学研究中的应用。

Determination of tamsulosin in human plasma by liquid chromatography/tandem mass spectrometry and its application to a pharmacokinetic study.

机构信息

School of Pharmacy, Sungkyunkwan University, Suwon 440-746, Republic of Korea.

出版信息

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.

Abstract

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.

摘要

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。

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