How can I reduce flash column purification time and cost?

This is a question being asked of my colleagues and me more and more frequently, especially in pharma accounts.  Why?  Well, you are familiar with the adage – Time is Money, right.  Well this really applies to them. A new molecular entity (NME) created as a pharmaceutical can take up to a decade and a billion dollars to bring to market.  Granted, the biggest costs are in the clinical trials but the synthetic route and the time to discover and make the compound – and purify it – plays a major role within drug discovery and development. This timeline is not helped by the ever increasingly difficult-to-synthesize compounds being investigated as drug candidates today.

With that in mind, this post focuses on ways to speed the purification process without sacrificing purity and yield. Continue reading How can I reduce flash column purification time and cost?

How can I perform normal-phase and reversed-phase column chromatography on one flash system?

For chemists, flash chromatography is part of their everyday synthesis workflow. For most syntheses, crude reaction mixtures are purified by normal-phase (aka adsorption) chromatography.  There are times; however, where the crude mixture’s complexity and polarity make normal-phase chromatography very challenging.  For these situations, reversed-phase (aka partition) chromatography may be a preferred option.

But, if you have only one flash system available, can you, should you, and how do you efficiently switch from non-polar, normal-phase solvents to polar, reversed-phase solvents – and back again without issues? In this post I’ll attempt to shed some light on the topic. 

Continue reading How can I perform normal-phase and reversed-phase column chromatography on one flash system?

How can I make purification of hard-to-separate compounds greener?

The planet’s population is growing, its resources are dwindling – this is a problem.  On top of that environmental contamination from myriad sources is only compounding the issue of available clean food and water.

As chemists, we contribute to this issue, to some degree, by performing reactions that generate chemical waste in the form of unwanted by-products and excess solvents from work-up and purification. What can we, as chemists, do to help reduce our so-called “carbon footprint”?

In this post, I discuss some ways to improve flash chromatography resource utilization, especially for hard separations.
Continue reading How can I make purification of hard-to-separate compounds greener?

How to efficiently scale-up flash column chromatography

For synthesis and medicinal chemists, compounds are typically made only once en route to a final product. Once that compound shows activity toward a particular target, then the synthesis is scaled up meaning that purification too requires scaling. The same is true in natural product research where once a high-value compound is isolated at small scale, there is a need to isolate it at larger scale.

Both of these scenarios can be problematic to scale-up/ process chemists when other, non-chromatographic purification techniques are not successful. When this happens, either a different synthetic route or extraction process is needed or large scale chromatography is employed. In this post, I will explain how flash chromatography can be successfully scaled while minimizing time and solvent consumption. Continue reading How to efficiently scale-up flash column chromatography

How can I rapidly remediate THC from CBD in my hemp extract using flash column chromatography?

Tetrahydrocannabinol, aka THC, is a hallucinogen found in cannabis and, to a lesser degree, in hemp.  Though THC is legal in some locations in the US and Canada, there is a growing market for its non-hallucinogenic cousin, cannabidiol (CBD), which has purported medical benefits.

The problem with isolating CBD from cannabis and hemp is contamination from THC, which is typically present at a moderate to high percentage. In this post, I will provide some insight into rapidly purifying CBD to remove THC. Continue reading How can I rapidly remediate THC from CBD in my hemp extract using flash column chromatography?