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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 >Determination of triapine, a ribonucleotide reductase inhibitor, in human plasma by liquid chromatography tandem mass spectrometry
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Determination of triapine, a ribonucleotide reductase inhibitor, in human plasma by liquid chromatography tandem mass spectrometry

机译：液相色谱串联质谱法测定人血浆中的三氮平（一种核糖核苷酸还原酶抑制剂）

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摘要

Triapine is an inhibitor of ribonucleotide reductase (RNR). Studies have shown that triapine significantly decreases the activity of RNR and enhanced the radiation-mediated cytotoxicity in cervical and colon cancer. In this work, we have developed and validated a selective and sensitive LC-MS/MS method for the determination of triapine in human plasma. In this method, 2-[(3-fluoro-2-pyridinyl)methylene] hydrazinecarbothioamide (NSC 266749) was used as the internal standard (IS); plasma samples were prepared by deproteinization with acetonitrile; tripaine and the IS were separated on a Waters Xbridge Shield RP18 column (3.5 mu m; 2.1 x 50 mm) using a mobile phase containing 25.0% methanol and 75.0% ammonium bicarbonate buffer (10.0 mm, pH 8.50; v/v); column eluate was monitored by positive turbo-ionspray tandem mass spectrometry; and quantitation of triapine was carried out in multiple-reaction-monitoring mode. The method developed had a linear calibration range of 0.250-50.0 ng/mL with correlation coefficient of 0.999 for triapine in human plasma. The IS-normalized recovery and the IS-normalized matrix factor of triapine were 101-104% and 0.89-1.05, respectively. The accuracy expressed as percentage error and precision expressed as coefficient of variation were +/- 6 and 8%, respectively. The validated LC-MS/MS method was applied to the measurement of triapine in patient samples from a phase I clinical trial. Copyright (c) 2015 John Wiley & Sons, Ltd.
机译：Triapine是核糖核苷酸还原酶（RNR）的抑制剂。研究表明，特里亚平显着降低了RNR的活性并增强了宫颈癌和结肠癌的辐射介导的细胞毒性。在这项工作中，我们已经开发并验证了选择性和灵敏的LC-MS / MS方法，用于测定人血浆中的Triapine。在该方法中，将2-[（（3-氟-2-吡啶基）亚甲基]肼基碳硫代酰胺（NSC 266749）用作内标（IS）;用乙腈脱蛋白制备血浆样品。在含有25.0％甲醇和75.0％碳酸氢铵缓冲液（10.0 mm，pH 8.50; v / v）的流动相中，在Waters Xbridge Shield RP18色谱柱（3.5微米; 2.1 x 50毫米）上分离三甲胺和IS。柱洗脱液采用正涡轮离子喷雾串联质谱法进行监测。并以多反应监测的方式对特里亚平进行定量。开发的方法的线性校准范围为0.250-50.0 ng / mL，人血浆中的三氮平的相关系数为0.999。三氮平的IS归一化回收率和IS归一化基质因子分别为101-104％和0.89-1.05。以百分比误差表示的精度和以变异系数表示的精度分别为+/- 6和8％。经过验证的LC-MS / MS方法用于I期临床试验患者样品中的Triapine的测量。版权所有（c）2015 John Wiley＆Sons，Ltd.

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