| Title: | Generic gas chromatography-flame ionization detection method for quantitation of volatile amines in pharmaceutical drugs and synthetic intermediates |
| Author(s): | Graffius GC; Jocher BM; Zewge D; Halsey HM; Lee G; Bernardoni F; Bu X; Hartman R; Regalado EL; |
| Address: | "Process Research & Development, MRL, Merck & Co., Inc., Rahway, NJ 07065, USA. Electronic address: gabriel_graffius@merck.com. Process Research & Development, MRL, Merck & Co., Inc., Rahway, NJ 07065, USA. Agilent Technologies, Incorporated, Wilmington, DE 19808, USA. Process Research & Development, MRL, Merck & Co., Inc., Rahway, NJ 07065, USA. Electronic address: erik.regalado@merck.com" |
| DOI: | 10.1016/j.chroma.2017.08.048 |
| ISSN/ISBN: | 1873-3778 (Electronic) 0021-9673 (Linking) |
| Abstract: | "Volatile amines are among the most frequently used chemicals in organic and pharmaceutical chemistry. Synthetic route optimization often involves the evaluation of several different amines requiring the development and validation of analytical methods for quantitation of residual amine levels. Herein, a simple and fast generic GC-FID method on an Agilent J&W CP-Volamine capillary column (using either He or H(2) as the carrier gas) capable of separating over 25 volatile amines and other basic polar species commonly used in pharmaceutical chemistry workflows is described. This 16min method is successfully applied to the analysis and quantitation of volatile amines in a variety of pharmaceutically-related drugs and synthetic intermediates. Method validation experiments showed excellent analytical performance in linearity, recovery, repeatability, and limit of quantitation and detection. In addition, diverse examples for the application of this method to the simultaneous determination of other amine-related chemicals in reaction mixtures are illustrated, thereby indicating that these GC-FID method conditions can be effectively used as starting point during method development for the analysis of other basic polar species beyond the validated list of amines described in this study" |
| Keywords: | "Amines/*analysis Chemistry, Pharmaceutical/*methods *Chromatography, Gas *Flame Ionization Pharmaceutical Preparations/*chemistry Basic compounds Capillary column Gas chromatography-flame ionization detector Method development Pharmaceutical analysis Vola;" |
| Notes: | "MedlineGraffius, Gabriel C Jocher, Brandon M Zewge, Daniel Halsey, Holst M Lee, Gary Bernardoni, Frank Bu, Xiaodong Hartman, Robert Regalado, Erik L eng Netherlands 2017/09/09 J Chromatogr A. 2017 Oct 6; 1518:70-77. doi: 10.1016/j.chroma.2017.08.048. Epub 2017 Aug 23" |
