测定片剂中 N-亚硝基托法替尼毒性的高效 LC-MS/MS 方法

IF 16.4 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY

Accounts of Chemical Research Pub Date : 2024-07-18 DOI:10.2174/0115734110304169240705112652

Chitra P, Premakumari KB, Arun Bhuvanendran

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引用次数: 0

摘要

背景和目的：制药公司必须遵守监管机构制定的规则，以监控药品是否受到亚硝胺污染。在药物制剂和物质的生产过程中可能产生的一种亚硝胺是 N-亚硝基托法替尼。亚硝胺是一种致癌污染物。控制药品和医疗用品中亚硝胺的含量至关重要。在本研究中，我们设计了一种简单、复杂的 LC-MS/MS 方法来分析托法替尼片剂中的 N-亚硝基托法替尼。材料与方法液相色谱-串联质谱（LC-MS/MS）实验在 Jade C18（5μ，150 x 4.6 mm）上进行了优化，混合溶剂采用 pH 3.2 的 10mM 乙酸铵和乙腈，流速为 1.0 mL。采用的质谱转换（m/z）为 275.3/149.1、275.3 /147.0 和 275.3/82.1：线性范围为 0.7 - 20.0 ng/mL，r2 为 0.9952。最低检测限（LOD）和定量限（LOQ）分别为 0.7 纳克/毫升和 1.0 纳克/毫升。回收重复性在规定范围内。结论新方法可有效定量托法替尼片剂样品中的 N-亚硝基托法替尼杂质，可用于常规分析。

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An Efficient LC-MS/MS Method for Determining N-nitroso Tofacitinib Toxicity In the Tablet Form

Background and Objective: Pharmaceutical companies must adhere to rules established by regulatory agencies in order to monitor pharmaceutical products for nitrosamine contamination. One type of nitrosamine that can arise during the manufacture of the drug’s formulation and substance is N-Nitroso Tofacitinib. One pollutant that causes cancer is nitrosamines. Controlling the amount of nitrosamines in pharmaceuticals and medical supplies is essential. In this study, we devised a straightforward, sophisticated LC-MS/MS approach to analyse N-Nitroso Tofacitinib present in Tofacitinib tablets. Materials and Methods: Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) experiments were optimised on Jade C18 (5μ, 150 x 4.6 mm), solvent mixture was operated in gradient program using 10mM ammonium acetate pH 3.2 and acetonitrile with 1.0 mL flow rate. Mass transition (m/z) 275.3/149.1, 275.3 /147.0, and 275.3/82.1 are used Results: The range of linearity is 0.7 - 20.0 ng/mL, with r2 of 0.9952. The Lowest Detection (LOD) and quantification (LOQ) were 0.7 ng/mL and 1.0 ng/mL respectively. The recovery repeatability was found to be within the specified range. Conclusion:: The new approach proved effective for quantifying N-Nitroso Tofacitinib impurity in Tofacitinib Tablet samples, indicating that it could be applied for regular analysis.

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.