Series 4 - Research Process

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4# Initiate the research


This section will ‘summarise’ what I am and will be doing in my research project based on the explanations I have delivered earlier. I am eager to explore the analysis of amines, specifically secondary amines, in the pharmaceutical sample matrix, which, surprisingly, has not had many similar published studies so far.

There are many amine varieties in nature, and considering the safety aspect, here are my several choices of amines (again, I will focus more on the secondary ones): Diethanolamine, Dipropylamine, Diethylamine, Dibutylamine, Diisopropylamine, Pyrrolidine, Piperidine, and N-methyl pyrrolidinone (NMP). While NMP is a tertiary amine, its presence should also be a warning due to its ability to generate secondary amine under certain conditions.

I created a model solution for the sample matrix comprising Active Pharmaceutical Ingredients (APIs) and excipients to mimic the characteristics of an actual tablet drug but directly in solution form. My model solution used common excipients for tablet making, including Microcrystalline cellulose, Lactose monohydrate, Hydroxypropyl methylcellulose, and Croscarmellose sodium. As for my choice of API, I used Ibuprofen (part of an analgetic class), considering this compound has no amine in the origin structure formula; hence, it is expected not to form nitrosamines – to avoid bias. 

Based on the analytical methods considerations in the previous section, I chose Gas Chromatography (GC) with a Mass Spectrometry (MS) detector for the instruments. I started my research project by developing and optimising this GC-MS method. Later, I will also perform the validation method to ensure data reliability.

Figure 1. Thermo Scientific Trace 1310 Gas Chromatography with ISQ Single Quadrupole Mass Spectrometry 

What concerns are involved in developing the method? What are the significant challenges? Are the results promising?




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