Welcome to the Biotage Flash Purification Blogs.

    TLC-based vs. Generic Gradients – Which Gives the Best Results?

    January 12, 2021 at 1:40 PM / by Bob Bickler posted in Chromatography Fundamentals, Green, Method development

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    Over the course of my career, I have had terrific interactions with a multitude of chemists discussing chromatography. When it comes to flash chromatography the approaches from these chemists ranged from running generic 0-100% ethyl acetate in hexane gradients to modeled gradients based on tribal knowledge for a type of synthetic molecule to always using TLC for method development to prep HPLC. Each of these techniques are used because they provide some level of success. To me, though, if I spend time and resources synthesizing a highly valuable and unique molecule, then I want to purify the reaction mixture with the best possible method.

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    Can Flash Chromatography be Green? Part 1

    January 4, 2021 at 2:30 PM / by Bob Bickler posted in Amine, Chromatography Fundamentals, Solvents, Green, Media and Resin

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    The term “Green Chemistry” has become a major part of the science community’s lexicon. When I think about green chemistry and its relationship to flash column chromatography I think of two specific areas where it applies...

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    Can Flash Column Chromatography be Green? Part 2

    January 4, 2021 at 2:28 PM / by Bob Bickler posted in Chromatography Fundamentals, Green

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    Applying green chemistry principals to flash purification is becoming increasingly important.  In this post, I discuss ways to make flash column chromatography greener by reducing solvent use through optimization of gradient shape.

    This is a follow-on to my earlier post where I presented some greener alternatives to DCM as a solvent in flash column chromatography.

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    Can reversed-phase flash column chromatography be greener?

    December 3, 2020 at 7:24 PM / by Bob Bickler posted in Reversed-phase, Green

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    In previous posts I offered some suggestions to improve the “greenness” of normal-phase flash purification.  As the use of reversed-phase flash purification has increased the past few years I thought I would explore how to potentially make it greener too.

    So, with that in mind, let's take a look at the use of acetone in place of acetonitrile as a reversed-phase flash chromatography solvent.

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    Invest 10 minutes on TLC and save a day of grief

    November 13, 2020 at 1:17 PM / by Bob Bickler posted in Chromatography Fundamentals, Green, TLC

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    Flash column chromatography is used by between 20 and 40 thousand organic synthesis chemists worldwide, an amazing number. For most of these chemists flash chromatography is an important part of their daily workflow but allocating time for good method development is often not considered, which can lead to less than ideal purification results.

    In this post I focus on how allocating just 10 minutes on thin-layer chromatography (TLC) for method development can save you a lot of grief later on.

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    How does reversed-phase flash chromatography compare to prep HPLC?

    March 26, 2020 at 2:42 PM / by Bob Bickler posted in Reversed-phase, Green, Sfär, Selekt, HPLC

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    For medicinal chemists, maximizing the synthetic yield of their newly created intermediate compound is their priority. More times than not, flash chromatography is used to purify these intermediate compounds to at least 80% purity. Final compounds, however, not only require high yield but maximum attainable purity, typically in excess of 95%. For this purity level, chemists will either send the reaction mixture to an in-house prep HPLC lab or perform their own preparative HPLC compound purification, if it is available in the lab.

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    How do I decide between normal- or reversed-phase flash column chromatography?

    December 30, 2019 at 4:49 PM / by Bob Bickler posted in Chromatography Fundamentals, Reversed-phase, Green, Normal Phase, Isolera, HPLC

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    Choosing a good purification strategy is an important for successful crude compound purification. A major factor in your strategy is choosing between normal-phase or reversed-phase chromatography.  How do you choose?

    In this post, I will provide some simple guidance on helping determine which route to take.

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    Pushing flash column chromatography loading limits

    December 30, 2019 at 3:39 PM / by Bob Bickler posted in Chromatography Fundamentals, Green, Sfär, Loading Techniques, Cost, Normal Phase, Pillar Page

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    A question I hear a lot from chemists is “how much can I load”. The answer is always “it depends on your separation quality”.  At that point I begin asking about the TLC data and purification goals. Purification goal setting should be your first step and the question to answer is – what do I need this purification to achieve? Is the goal high purity, high yield, or some combination.  Remember, you will typically sacrifice purity for high yield and yield for high purity so optimization is an important consideration.

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    Green Flash Chromatography Webinar

    November 26, 2019 at 9:03 PM / by Bob Bickler posted in Green, Sfär, Selekt, Webinar, Cost, Normal Phase

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    Over the past several decades, the chemical industry has implemented process changes and updated practices in R&D and manufacturing in an effort to reduce liquid and solid lab waste. The pharmaceutical industry in particular has taken steps within their drug discovery labs to reduce solvent use by requiring their chemists to find and implement measures that achieve the corporate environmental goals without curtailing their productivity – quite the challenge.

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    How do I purify ionizable organic amine compounds using flash column chromatography?

    November 21, 2019 at 3:59 PM / by Bob Bickler posted in Amine, Chromatography Fundamentals, Solvents, Troubleshooting and Optimization, Green, Media and Resin

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    For most organic reaction mixture purifications the process is fairly straightforward. Use hexane/ethyl acetate or, for polar compounds, DCM/MeOH.  But what do you do if this doesn't work and your compounds are basic organic amines?

    In this post, I re-examine the options available to achieve an acceptable organic amine purification when typical separation methods are insufficient.

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    How Much Is My Flash Chromatography System Really Going to Cost?

    November 15, 2019 at 3:01 PM / by John Urh posted in Solvents, Green, Cost

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    This, of course, is always one of the first questions an organic, medicinal, or peptide chemist has when starting the research process for a flash chromatography system. Here at Biotage, we receive this question hundreds and hundreds of times a year, likely within the first couple of minutes of any conversation.

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    The Step Gradient Explained

    November 1, 2019 at 9:37 PM / by Greg Saunders posted in Chromatography Fundamentals, Solvents, Green, Cost, Normal Phase, Isolera

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    Up to six compounds can be easily separated with an automated step-gradient optimizer embedded in modern flash chromatography systems.

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    What if you could use Semi-Preparative HPLC columns on your Flash Chromatography system?

    October 24, 2019 at 2:08 PM / by Panagiotis Ioannidis posted in Reversed-phase, Green, Selekt, Cost, HPLC

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    The newly released Biotage® Selekt flash chromatography instrument can be run at a maximum flow-rate of 300 mL/min or a maximum pressure of 30 bar. These high flowrates and pressures enable a user to perform chromatography using not only dry-packed, single-use plastic flash columns containing small (≥20 μm) spherical silica particles, but also semi-preparative, slurry-packed
    HPLC columns for multiple use with smaller (≤20 μm) spherical silica particles.

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    What is a Chromatography Gradient?

    October 2, 2019 at 3:27 PM / by Bob Bickler posted in Chromatography Fundamentals, Green, Sfär, Selekt, Normal Phase

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    Gradients, used in chromatographic methods, assist with chemical separation and elution. They begin with “weak” elution conditions and end with “strong” elution conditions.

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    How do I Choose the Right Column Size for Purification by Flash Chromatography?

    June 13, 2019 at 4:59 PM / by Bob Bickler posted in Chromatography Fundamentals, Green, Scale-Up

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    In all my years of working with medicinal and organic chemists, I have found that choosing how many grams of silica to use for purification by flash chromatography is something frequently guessed at. Getting the size of the column right is awfully important because using too few grams of silica will doom your purification to failure and using more an optimal mass of the stationary phase means the purification consumes excess silica, solvents, and a chemist's time.

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    How many ways can you load sample on your column?

    May 31, 2019 at 4:02 PM / by Raffaella Bombarda posted in Chromatography Fundamentals, Green, Sfär, Loading Techniques, Scale-Up

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    Biotage®, a pioneer in Flash Purification, launched the unique, removable cap SNAP flash chromatography columns in 2007. This beneficial column design feature continues with the newest Biotage flash columns named Sfär columns.

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