A day in the life of a chiral sample.

A day in the life of a chiral sample - 12th September 2014
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 to us. The entire lab team then receives an alert regarding the incoming sample immediately, allowing them to allocate resources efficiently.

An Agilent 1100 LCMS fitted with diode array detection (DAD) records the chemical purity. A gradient method is performed on a C18 column and the UV trace, TIC are recorded and the lambdamax and molecular weight determined. This is then uploaded to the sample area, allowing our clients to see our initial purity data.

Each sample is then screened across normal phase, polar organic, reversed phase HPLC and SFC. This occurs in parallel, usually overnight in order to maximise capacity. Once a method has been found it is developed by one of the team and transferred straight to preparative scale on either one of the three Berger Multi Gram preparative SFC systems or one of four chiral Gilsons.

Our Gilson HPLC systems are adapted specifically for enantiomeric and diastereomeric separations, collecting in timed windows into durans, virtually eliminating the possibility of human error during fraction manipulation (see this blog for more details). Whether by HPLC or SFC, a method will be found incorporating stacked injections to ensure a high quality separation in an efficient manner in order to meet Reach’s self-imposed strict deadlines.

Post purification fractions are combined and dried using a rotary evaporator. At this stage they are reanalysed on both the developed chiral method and a reversed phase achiral method. This ensures the chiral specification has been met and that the chemical purity has not been compromised during the chiral separation.

Once analysis has been carried out the samples are transferred in DCM to pre-tared vials and the analysis checked once more. This final quality data is uploaded to the secure submission and reporting system.

The samples are placed in a vacuum oven overnight, and dried to a constant weight. The final report is then compiled and the samples are finally dispatched back to the client using a fast and reliable courier service.

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.


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