基于质谱的分析程序的性能特征用于药品中氨酸的量化:从实验室间研究的见解
Jingyue Yang1, Raghavi Kakarla1, Tim Marzan1
1Office of Testing and Research, Center of Drug Evaluation and Research, US Food and Drug Administration, Saint Louis, MO 63110, USA.
Journal of pharmaceutical sciences
|July 31, 2023
概括
药品中致癌性尼托拉胺杂质的有效测试至关重要. 一项实验室间的研究证实,质谱仪在各种分析方法中准确量化这些微量污染物.
科学领域:
- 制药分析 制药分析
- 分析化学是一种分析化学.
- 监管科学是一种监管科学.
背景情况:
- 2018年,在药品中发现了致癌的尼托胺杂质.
- 监管机构现在要求对尼托胺的形成进行风险评估.
- 确保药品质量需要有效的尼托胺测试.
研究的目的:
- 为了评估测量变化在尼托胺的确定.
- 评估尼托胺测试分析程序的性能.
- 提供对质谱仪用于微量尼托胺分析的能力的见解.
主要方法:
- 进行了一项涉及六个监管机构实验室的实验室间研究.
- 参与者使用他们自己的分析程序来测试相同的样本.
- 质谱是用于检测和量化的主要技术.
主要成果:
- 通过精确和精确的量化,可以实现微量尼托胺的量化.
- 结果在多种多样化的分析程序中一致.
- 评估了质谱仪的性能特征 (准确性,可重复性,可重复性).
结论:
- 基于质谱的方法是可靠的量化药品中微量尼托胺.
- 实验室间的研究对于评估分析方法的性能非常有价值.
- 标准化或验证的方法可以确保药物安全的一致的质量控制.
更多相关视频
08:41Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications
Published on: July 14, 2017
9.4K
07:14Automated, High-resolution Mobile Collection System for the Nitrogen Isotopic Analysis of NOx
Published on: December 20, 2016
11.7K
相关概念视频
Atomic Absorption Spectroscopy: Lab
479
For AAS measurements, samples must be introduced as clear solutions, often requiring extensive preliminary treatment to dissolve materials like soils, animal tissues, and minerals. Common methods for sample preparation include treatment with hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, or fusion with reagents.
Solutions containing organic solvents, such as low-molecular-mass alcohols, esters, or ketones, enhance absorbances by increasing...
Solutions containing organic solvents, such as low-molecular-mass alcohols, esters, or ketones, enhance absorbances by increasing...
479
2° Amines to N-Nitrosamines: Reaction with NaNO2
4.3K
Secondary amines react with nitrous acid to form N-nitrosamines, as depicted in Figure 1. Nitrous acid, a weak and unstable acid, is formed in situ from an aqueous solution of sodium nitrite and strong acids, such as hydrochloric acid or sulfuric acid, in cold conditions. In the presence of an acid, the nitrous acid gets protonated. The subsequent loss of water results in the formation of the electrophile known as nitrosonium ion.
4.3K
Mass Spectrometry of Amines
4.2K
In mass spectroscopy, amines undergo fragmentation to give parent ions with odd molecule weights. This observed mass spectrum follows the nitrogen rule: a molecule with an odd number of nitrogen atoms produces a parent ion with an odd molecular weight. The remaining fragments have an even mass.
Amines undergo fragmentation through α cleavage, producing nitrogen-containing cations—iminium ions—and alkyl radicals. Mass spectra of aromatic and cyclic aliphatic amines exhibit...
Amines undergo fragmentation through α cleavage, producing nitrogen-containing cations—iminium ions—and alkyl radicals. Mass spectra of aromatic and cyclic aliphatic amines exhibit...
4.2K
