高灵敏的二维离子染色学质谱法,用于化甲基纤维素中酸盐的测定
Koudi Zhu1, Michael Kerry2, Barbara Serr2
1Pharma Solutions, IFF, Midland, MI 48640, USA; Department of Chemical Engineering, Vrije Universititeit Brussel, Pleinlaan 2, Brussel 1050, Belgium.
Journal of pharmaceutical and biomedical analysis
|July 9, 2024
概括
这项研究开发了一种敏感的二维离子染色学质谱 (2D-IC/MS) 方法,用于在HPMC等药物辅助剂中确定微量酸盐,这对于控制尼托胺药物杂质至关重要.
科学领域:
- 分析化学 分析化学
- 制药科学 制药科学
背景情况:
- 药物中的氨酸具有健康风险,并且由于潜在的致癌性而受到监管.
- 尼胺的形成与制药助剂中酸盐的存在有关.
- 在辅助剂中精确的微量酸盐测定对于药物安全性和供应商选择至关重要.
研究的目的:
- 开发和验证一种敏感的分析方法,用于在基甲基纤维素 (HPMC) 中测定微量酸盐.
- 为了使药品制造商能够评估辅助剂的质量,并减轻尼托胺的风险.
主要方法:
- 开发一种使用心脏切割模式的二维离子染色体质谱 (2D-IC/MS) 方法.
- 使用度柱,离子交换柱 (1D和2D),以及用同位素标记的内部标准进行质谱检测.
- 实施了一种新的实验室用品清洁程序,以消除酸盐污染.
主要成果:
- 2D-IC/MS方法在HPMC中实现了对微量酸盐检测的高灵敏度和特异性.
- 验证了线性 (R2 > 0.9999),精度 (RSD 3.5-10.1%) 和恢复 (90.5-102.4%).
- 在HPMC中达到8.9 ng/g的检测极限和29.6 ng/g的量化极限.
结论:
- 开发的2D-IC/MS方法适用于药品辅助剂中敏感且准确的微量亚酸盐的确定.
- 这种方法支持制药行业控制尼托胺杂质,并确保药物产品的安全.
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