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首页> 外文期刊>Journal of Pharmaceutical Analysis >Sensitive and rapid determination of amantadine without derivatization in human plasma by LC–MS/MS for a bioequivalence study
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Sensitive and rapid determination of amantadine without derivatization in human plasma by LC–MS/MS for a bioequivalence study

机译：LC-MS / MS灵敏快速测定人血浆中金刚烷胺而不衍生化，用于生物等效性研究

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A highly sensitive, rapid and rugged liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS) method was developed for reliable estimation of amantadine (AMD), an antiviral drug in human plasma. The analyte and internal standard (IS), amantadine-d6?(AMD-d6), were extracted from 200?μL plasma by solid phase extraction on Phenomenex Strata-X-C 33?μ cartridges. Chromatography was performed on Synergi? Hydro-RP C18(150?mm × 4.6?mm, 4?μm) analytical column using a mixture of acetonitrile and 10?mM ammonium formate, pH 3.0 (80:20, v/v) as the mobile phase. Detection and quantitation was done by multiple reaction monitoring in the positive ionization mode for AMD (m/z152.1 → 135.1) and IS (m/z158.0 → 141.1) on a triple quadrupole mass spectrometer. The assay was linear in the concentration range of 0.50–500?ng/mL with correlation coefficient (r2) ≥ 0.9969. The limit of detection of the method was 0.18?ng/mL. The intra-batch and inter-batch precisions were ≤ 5.42% and the accuracy varied from 98.47% to 105.72%. The extraction recovery of amantadine was precise and quantitative in the range of 97.89%–100.28%. IS-normalized matrix factors for amantadine varied from 0.981 to 1.012. The stability of AMD in whole blood and plasma was evaluated under different conditions. The developed method was successfully applied for a bioequivalence study with 100?mg of AMD in 32 healthy volunteers. The reproducibility of the assay was determined by reanalysis of 134 subject samples.
机译：开发了一种高度灵敏，快速而坚固的液相色谱-串联质谱（LC-ESI-MS / MS）方法，用于可靠地估算人血浆中的抗病毒药物金刚烷胺（AMD）。在Phenomenex Strata-X-C 33？μ柱上通过固相萃取从200？L血浆中提取了分析物和内标（IS），金刚烷胺-d6？（AMD-d6）。色谱法在Synergi？上进行。 Hydro-RP C18（150？mm×4.6？mm，4？μm）分析柱，使用乙腈和10？mM甲酸铵，pH 3.0（80:20，v / v）的混合物作为流动相。通过在三重四极杆质谱仪上以正离子化模式对AMD（m / z152.1→135.1）和IS（m / z158.0→141.1）进行多反应监测来进行检测和定量。该测定在0.50–500？ng / mL的浓度范围内呈线性，相关系数（r2）≥0.9969。该方法的检出限为0.18？ng / mL。批内和批间精度≤5.42％，精度从98.47％到105.72％不等。金刚烷胺的提取回收率精确且定量，范围为97.89％–100.28％。金刚烷胺的IS归一化矩阵因子从0.981到1.012。在不同条件下评估了AMD在全血和血浆中的稳定性。所开发的方法已成功应用于32名健康志愿者中100 mg的AMD的生物等效性研究。通过对134个受试者样品进行重新分析来确定测定的可重复性。

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