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采用 HPLC-MS/MS 法对人血浆中的埃利替坦进行定量分析及其在药代动力学研究中的应用。

Quantitative analysis of eletriptan in human plasma by HPLC-MS/MS and its application to pharmacokinetic study.

机构信息

Chalapathi Institute of Pharmaceutical Sciences, Lam, Guntur, Andhra Pradesh 522034, India.

出版信息

Anal Bioanal Chem. 2011 Nov;401(8):2539-48. doi: 10.1007/s00216-011-5341-4. Epub 2011 Sep 3.

DOI:10.1007/s00216-011-5341-4
PMID:21892641
Abstract

Authors developed a simple, sensitive, selective, rapid, rugged, and reproducible liquid chromatography-tandem mass spectrometry method for the quantification of eletriptan (EP) in human plasma using naratriptan (NP) as an internal standard (IS). Chromatographic separation was performed on Ascentis Express C18, 50 × 4.6 mm, 2.7 μm column. Mobile phase was composed of 0.1% formic acid: methanol (40:60 v/v), with 0.5 mL/min flow rate. Drug and IS were extracted by liquid-liquid extraction. EP and NP were detected with proton adducts at m/z 383.2→84.3 and 336.2→97.8 in multiple reaction monitoring (MRM) positive mode, respectively. The method was validated with the correlation coefficients of (r(2)) ≥ 0.9963 over a linear concentration range of 0.5-250.0 ng/mL. This method demonstrated intra- and inter-day precision within 1.4-9.2% and 4.4-5.5% and accuracy within 96.8-103% and 98.5-99.8% for EP. This method is successfully applied in the bioequivalence study of 24 human volunteers.

摘要

作者开发了一种简单、灵敏、选择性好、快速、稳健且重现性佳的液质联用法,用于人血浆中依来曲普坦(EP)的定量分析,内标物为那拉曲坦(NP)。色谱分离在 Ascentis Express C18 柱(50×4.6mm,2.7μm)上进行,流动相由 0.1%甲酸-甲醇(40:60,v/v)组成,流速为 0.5mL/min。采用液液萃取法提取药物和内标物。EP 和 NP 采用正离子多反应监测(MRM)模式,以质子加合物形式检测,m/z 分别为 383.2→84.3 和 336.2→97.8。该方法在 0.5-250.0ng/mL 的线性浓度范围内,相关系数(r(2))均≥0.9963。该方法在 EP 分析中表现出日内和日间精密度分别为 1.4-9.2%和 4.4-5.5%,准确度分别为 96.8-103%和 98.5-99.8%。该方法成功应用于 24 名健康志愿者的生物等效性研究。

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