一种用于检测和定量药用辅料中甲醛杂质的稳健静态顶空气相色谱 - 火焰离子化检测法 - Suppr

A Robust Static Headspace GC-FID Method to Detect and Quantify Formaldehyde Impurity in Pharmaceutical Excipients.

作者信息

Daoud Agha Dit Daoudy Bashir, Al-Khayat Mohammad Ammar, Karabet Francois, Al-Mardini Mohammad Amer

机构信息

Department of Pharmaceutical Chemistry and Quality Control, Faculty of Pharmacy, Damascus University, Damascus, Syria.

Department of Chemistry, Faculty of Science, Damascus University, Damascus, Syria.

出版信息

J Anal Methods Chem. 2018 Mar 4;2018:4526396. doi: 10.1155/2018/4526396. eCollection 2018.

Formaldehyde is a highly reactive impurity that can be found in many pharmaceutical excipients. Trace levels of this impurity may affect drug product stability, safety, efficacy, and performance. A static headspace gas chromatographic method was developed and validated to determine formaldehyde in pharmaceutical excipients after an effective derivatization procedure using acidified ethanol. Diethoxymethane, the derivative of formaldehyde, was then directly analyzed by GC-FID. Despite the simplicity of the developed method, however, it is characterized by its specificity, accuracy, and precision. The limits of detection and quantification of formaldehyde in the samples were of 2.44 and 8.12 g/g, respectively. This method is characterized by using simple and economic GC-FID technique instead of MS detection, and it is successfully used to analyze formaldehyde in commonly used pharmaceutical excipients.

甲醛是一种高活性杂质，在许多药用辅料中都能发现。这种杂质的痕量水平可能会影响药品的稳定性、安全性、有效性和性能。开发并验证了一种静态顶空气相色谱法，用于在使用酸化乙醇进行有效衍生化程序后测定药用辅料中的甲醛。然后通过气相色谱 - 火焰离子化检测器（GC - FID）直接分析甲醛的衍生物二乙氧基甲烷。然而，尽管所开发的方法很简单，但其具有特异性、准确性和精密度的特点。样品中甲醛的检测限和定量限分别为2.44和8.12 μg/g。该方法的特点是使用简单且经济的GC - FID技术而非质谱检测，并且已成功用于分析常用药用辅料中的甲醛。