The Life of a Chiral Sample!

In any given week Reach Separations can get up to 20 samples entering the lab. The life of a sample here at Reach is a short but interesting one. This is the story of a standard sample for chiral purification as it passes through one of our laboratories.

The journey begins when a client registers a sample using our online submission and reporting system; this is a quick and secure way for our clients to transfer all sample information. Once a sample is submitted, the senior lab team start to plan resources appropriately, ensuring racemates are processed and isomers returned to clients as quickly as possible.

On arrival all samples go straight to our analytical laboratory and into the safe hands of our dedicated QC Analyst. All incoming samples are analysed on a Waters HClass UHPLC and the incoming purity recorded before the chiral screen begins. We have more than 100 chiral methods available here at Reach HQ, utilising different techniques, stationary phases and mobile phases. We take advantage of the fast equilibration times and green credentials of Supercritical Fluid Chromatography (SFC) as well as more traditional High Performance Liquid Chromatography (HPLC). Our automated analytical instruments run through the night to ensure we find methods as quickly as possible.

Once a suitable stationary phase and mobile phase has been found, the method is optimised and purification can begin. We have a range of purification kit suitable for all of the samples we see here at Reach, form 10mg to 1kg! Each instrument is capable of stacked injections, speeding up purification and allowing us to return isomers within just a few days of receipt.

Stacked injections allow us to be using all of the stationary phase available in the column, all of the time. This example shows 300mg of racemate being processed in less than 25 minutes.

Post purification fractions are combined and dried using a rotary evaporator. For large scale separations we utilise automated rotary evaporators which can continue through the night. Quick purity checks are carried out now, before isomers are transferred into final vessels. If a specification is unusually high (>99EE) or we couldn’t fully resolve the isomers, an isomer may undergo a secondary purification at this point.

Final samples are then transferred and solvent removed on the Biotage VI0, before final analysis is obtained and the isomers stored in the vacuum oven overnight, dried to a constant weight.

A comprehensive report containing purity values, gross/tare weights, chromatograms, method details and preparative screenshots is written and available electronically whilst the isomers are packaged and returned to the client, allowing them to progress their project.

Depending on the amount of material, its lifetime at Reach Separations can be anything from one day to two weeks. Typically we aim to return five grams or less inside of five working days. However, the scientists at Reach will always endeavour to return the sample to the client as quickly as possible.