通过GC-MS/MS与Headspace模块与Autosampler溶剂通风模式同时确定六种不同药物剂量形式的尼胺:开发和验证
Hayriye İçin1, Hasan Tünel2, Hakan Akbıyık2
1Istanbul Technical University, Faculty of Science, Chemistry Department, Istanbul, Türkiye; Abdi Ibrahim Pharmaceuticals R&D Centre, Istanbul, Türkiye.
概括
一种新的分析方法可以准确地确定制药产品中的六种亚胺,克服矩阵效应. 这种经过验证的方法通过在FDA定义的限度内量化杂质来确保药物安全.
科学领域:
- 药品分析 药品分析
- 分析化学 分析化学
- 药品安全 药品安全
背景情况:
- N-尼托胺是制药药品中的关键杂质.
- 准确量化尼托胺对于确保患者安全至关重要.
- 现有的方法可能会面临各种药物配方的矩阵效应的挑战.
研究的目的:
- 开发和验证一种可靠的分析方法,用于确定各种药物剂量形式的六种特定的尼托胺.
- 消除矩阵效应,以准确量化N-二甲基胺 (NDEA),N-二甲基胺 (NDMA),N-二甲基胺 (NDIPA),N-二甲基胺 (NMPA),N-二甲基胺 (NEIPA) 和N-二甲基胺 (NDBA).
- 根据FDA关于可接受的每日摄入量的指导来确定度限制.
主要方法:
- 在悬浮剂,乳液和片剂形式的六种亚胺的量化.
- 使用气相色谱 (GC) 具有MS/MS检测器和Headspace (HS) 模块.
- 采用VF-WAXMS毛细管柱,并与GC-MS/MS自取样方法进行验证.
主要成果:
- 该方法表现出极好的线性 (R2 > 0.99),准确性 (79.5-122.4%的回收率) 和精度 (RSD < 15.0%).
- 成功量化了由FDA指导方针产生的既定度限制内的尼托胺.
- 开发的方法有效地减轻了不同药物形式的干扰矩阵效应.
结论:
- 经过验证的分析方法提供了准确可靠的药品中氨酸的确定.
- 这种方法有助于提高药物安全性,通过允许精确的杂质分析.
- 这种方法适用于药品配方的常规质量控制,以检查尼托胺污染.
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