A purification strategy for a medicinal chemistry group at Boehringer Ingelheim in Vienna, Austria, using the Agilent 1100 Series purification system was developed. The goal was to develop a simple purification process, which could be easily used by all chemists. Further challenges were to develop a set of pre-defined methods to purify not only simple samples but also problematic samples, such as insoluble samples, polar samples and samples that show poor ionization.
This document details the development of a simple, walk-up workflow for preparative HPLC-MS purification at Boehringer Ingelheim. The strategy utilizes the Agilent 1100 Series purification system to handle standard samples as well as problematic ones, such as insoluble, polar, and poorly ionizing compounds.
The note outlines five specific pre-defined methods suitable for different sample characteristics. It demonstrates a real-life application where these methods were used to separate cis/trans isomers from a crude reaction mixture, successfully isolating pure fractions.
| Column ID | 21.2-mm id. |
|---|---|
| Flow rate | 20 mL/min |
| Maximum sample load | 50 mg per injection |
| Standard sample volume | 500 pL |
| Column temperature | ambient |
The maximum sample load should be no more than 50 mg per injection.
Insoluble samples are dissolved in 500 pL of DMSO.
A set of five pre-defined methods was generated for different sample types.