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首页> 外文期刊>Biomedical Chromatography: An International Journal Devoted to Research in Chromatographic Methodologies and Their Applications in the Biosciences >Ultra-performance liquid chromatography-tandem mass spectrometric assay for the simultaneous determination of brucine, strychnine and brucine N-oxide in rat plasma: application to a pharmacokinetic study
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Ultra-performance liquid chromatography-tandem mass spectrometric assay for the simultaneous determination of brucine, strychnine and brucine N-oxide in rat plasma: application to a pharmacokinetic study

机译：超高效液相色谱-串联质谱测定法同时测定大鼠血浆中的苯丙氨酸，士丁碱和苯丙氨酸氮氧化物：在药代动力学研究中的应用

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A rapid, simple and sensitive UHPLC-MS/MS method was developed and validated for the simultaneous determination of brucine, strychnine and brucine N-oxide in rat plasma using huperzine A as an internal standard (IS) after protein precipitation with methanol. The analytes were separated on a Purospher (R) STAR RP18 UHPLC column (2 mu m, 2.1x100mm) by gradient elution using a mobile phase composed of methanol and water (containing 0.1% formic acid) at a flow rate of 0.3mL/min. Brucine, strychnine, brucine N-oxide and IS were detected in positive ion multiple reaction monitoring mode by means of an electrospray ionization interface (m/z 395.2324.1, m/z 335.2184.1, m/z 411.2394.2, m/z 243.1226.1). The calibration curve was linear over the range of 1-500ng/mL for brucine and strychnine and 0.2-50ng/mL for brucine N-oxide. The intra- and inter-day precisions of these analytes were all within 15% and the accuracy ranged from 85 to 115%. The stability experiment indicated that the plasma samples at three concentration levels were stable under different conditions. The developed method was successfully applied for the first time to pharmacokinetic studies of brucine, strychnine and brucine N-oxide following a single oral and intravenous administration of modified total alkaloid fraction in rats. Copyright (c) 2016 John Wiley & Sons, Ltd.
机译：建立了一种快速，简单且灵敏的UHPLC-MS / MS方法，并验证了使用石杉碱A作为内标（IS）甲醇沉淀后，可同时测定大鼠血浆中的铍，士丁碱和铍N-氧化物。通过使用由甲醇和水（含0.1％甲酸）组成的流动相，以0.3mL / min的流速进行梯度洗脱，在Purospher（R）STAR RP18 UHPLC色谱柱（2μm，2.1x100mm）上分离分析物。通过电喷雾电离界面（m / z 395.2324.1，m / z 335.2184.1，m / z 411.2394.2，m / z z 243.1226.1）。丁香碱和士的宁的校准曲线在1-500ng / mL范围内线性，而丁香碱N-氧化物的校准曲线在0.2-50ng / mL范围内。这些分析物的日内和日间精度均在15％以内，精度范围为85至115％。稳定性实验表明，三种浓度水平的血浆样品在不同条件下均稳定。在大鼠口服和静脉内施用修饰的总生物碱成分后，该开发的方法成功地首次成功地应用于了苯丙氨酸，士的宁和苯丙氨酸N-氧化物的药代动力学研究。版权所有（c）2016 John Wiley＆Sons，Ltd.

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