Biotage Application Notes purification, Flash Chromatography

Application Notes- Purification

Novel Isolera Gradient Optimization Feature Reduces

Solvent Consumption, Waste, and Operating Costs
A major cost for synthetic chemistry laboratories is solvent, especially solvent used for compound purification. As companies look to decrease operating costs, this expense is being targeted and ways to reduce expenditures sought.

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Eliminating Aqueous Work-Up in Multiple Step Solution-Phase Synthesis using Flash Chromatography
Solution-phase synthetic techniques offer many advantages over solid-phase approaches such as unlimited scale, easy manipulation, and reduction in validation time. Recently the use of solution-phase chemistry for library generation has received increased attention as a lead investigation and optimization tool in drug discovery.

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Using TLC to Accurately Predict FLASH Purification Results
Thin-layer chromatography (TLC) is a commonly used method development tool for flash purification. Product mixtures separated using TLC generally can be purified by flash chromatography using the identical solvent system.

Download Application Note 42 (PDF - 144 kB)

Improving Reversed-Phase FLASH Purification Throughput
For many synthesized products purification on standard flash silica is not an option due to irreversible adsorption, chemical interaction
and/or solubility issues. Reversed-phase flash purification is an excellent solution for these applications.

Download Application Note 41 (PDF - 269 kB)

Increasing Purification Efficiency By Media Type Optimization
To increase purification efficiency, different media types including polymeric adsorbents HP20SS, XAD-1180, and a reversed-phase C18 (KP-C18-HS) were evaluabed. A Biotage FLASH purification system, driven by positive pressure, was used to optimize the separation conditions for this antibiotic. The optimization process focused on increasing sample loading capacity, purity, yield and elution linear velocity.

Download Application Note 39 (PDF - 569 kB)

Continuous Gradient Purification of Closely Related Drug Intermediates Using Flash Chromatography
In the early nineties, Biotage, Inc., developed the concept of a disposable FLASH chromatography cartridge to simplify and improve standard laboratory-scale flash purification. Since then, Biotage has continuously enhanced the purification process by developing novel products that provide unique solutions to challenging purification problems. In this study, a new normal-phase gradient elution technique has been developed, which minimizes TLC method development.

Download Application Note 38 (PDF - 1 094 kB)

Solvent Modification for Optimal FLASH-AC™ Carbon Purification Performance
Activated carbon is an adsorbent media used to remove colored compounds from solution. Using carbon in a packed bed, such as the Biotage FLASH-AC cartridge improves adsorbent performance. The key variable in optimizing the decolorization process is the solvent system. Varying the solvent system impacts the adsorbent capacity of the cartridge, affecting both the yield and purity of the product.

Download Application Note 37 (PDF - 258 kB)

Heated Solutions for Optimal FLASH-AC™ Carbon Purifcation Performance
This application compares the performance of Biotage FLASH-AC cartridges at room and high remperature. This study also shows how temperature is a process variable that may contribute to significan process improvement and reduce the total cost of operation.

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FLASH Purification in Lithium Aluminum Hydride Reduction of Carboxylic Acid
This paper describes a fast convenient isolation of 9- xanthenemethanol (2) formed from LiAIH4 reduction of xanthenemethanol 9-carboxylic acid by using the Biotage FLASH 12i/40i system with a Sample Injection Modular (SIM).

Download Application Note 35 (PDF - 326 kB)

Purifying Solution-Based Synthetic Peptides with FLASH Chromatography
Successful synthesis of a protein or a large peptide chain requires rapid and efficient purification. Fully protected peptides are difficult to isolate and purify because of their hydrophobic and bulky nature. With rapid purification, the protected peptides do not degrade and their recovery, yield and purity are usually very high.

Download Application Note 34 (PDF - 131 kB)

Reversed-phase FLASH Purification of a Synthetic Antibiotic Precursor by Quad UV™
This application note discusses how the new, automated Quad UV Parallel FLASH Purification system with in-line UV detection and automated fraction collection is used to purify, identify and collect the isomers of an aqueous modified antibiotic precursor. The goal for this work was to isolate each isomer with > 98% purity.

Download Application Note 33 (PDF - 130 kB)

Integrating Organic Synthesis and Purification Synthesis Optimization of Dicyclopropylmethyl Derivatives
This work introduces a new synthesis technique (Syn-FLASH) that streamlines the post reaction process by combining the synthesis, post-reaction work-up and purification process. Syn-FLASH minimizes the chance for chemical spills and fires while reducing on-column decomposition of sensitive compounds. Syn-FLASH also allows the recovery of starting materials and reagents.

Download Application Note 30 (PDF - 124 kB)

Purification of 9-Fluorenylmethanol Comparison of FLASH and Crystallization Purification Techniques
This paper compares crystallization of FLASH chromatography purification using prepacked cartridges. To compare both techniques, 9-Fluorenylmethanol (FmOH) is purified and the final product yield, solvent, time and the ease of scaling-up are compared.

Download Application Note 29 (PDF - 125 kB)

Performance of Parallex Flex™ HPLC
Parallel Flex is a preparative, high-performance liquid chromatography (HPLC) system that can be configured from one to four independent flow paths - eliminating the purification bottleneck in the process of drug discovery. The Flex system has been used by many pharmaceutical companies to purify compounds in the process of drug discovery.

Download Application Note 28 (PDF - 82 kB)

FLASH Purification of a Macrolide Antibiotic Extract Using In-line UV Detection
This application note discusses how the new, automated Quad UV Parallel FLASH Purification system with in-line UV detection and fraction collection is used to purify, collect and identify the various avermectin components in a semi-synthetic extract.

Download Application Note 27 (PDF - 109 kB)

Parallel Synthesis and Purification of Monoterpenoid Esters by Parallex Flex™ HPLC
In this study, a series of monoterpenoid esters, including 27 compounds, were synthesized using parallel synthesis techniques. This group of compounds will be used for further screen assays and chemical characterization. Both screen assay and chemical characterization require the purified compounds to be delivered in a timely manner.

Download Application Note 26 (PDF - 407 kB)

Improving Natural Product Purity by Orthogonal FLASH Purification
In this application, several solvent systems were evaluated by TLC. No solvent system was capable of resolving capsaicin, dihydrocapsaicin and lutein from each other. The best solvent mixture for this TLC separation was 90:10 methylene chloride (DCM)/ acetonitrile (ACN).

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Effects of Solvent Type and Strength in FLASH™ Separations
This application note shows how utilizing TLC (thin layer chromatography) with different solvent mixtures and polarities results in better FLASH separations of structurally similar compounds in less than 30 minutes. This work also shows how the TLC scouting results translate to FLASH separations and how they are used to optimize the separation of up to 12 different samples simultaneously.

Download Application Note 21 (PDF - 317 kB)

Analysis and Purification of Combinatorial Arrays by Reversed Phase FLASH™
This work illustrates how C18 reversed phase FLASH cartridges are used to monitor the reaction's progress and to isolate the products from the reaction mixture.

Download Application Note 17 (PDF - 744 kB)

High Speed Flash Fractionation of Natural Products - Tocopherols
Using reversed phase flash chromatography as the preliminary isolation step allows the tocopherols to be concentrated and have fewer oil contaminants thereby increasing the lifetime of the HPLC columns.

Download Application Note 16 (PDF - 505 kB)

High Speed Flash Fractionation of Natural Products - Polyphenols
Using reversed phase flash chromatography as the preliminary isolation step allows the tocopherols to be concentrated and have fewer oil contaminants thereby increasing the lifetime of the HPLC columns.

Download Application Note 15 (PDF - 349 kB)

Separation of Synthetic Organic Mixtures by Flash Chromatography
This work illustrates how quick and easy it is to include a flash purification step to isolate individual compounds from a single pot reaction mixture.

Download Application Note 14 (PDF - 466 kB)

A New Strategy to Isolate Combinatorial Array with the Quad3™ FLASH System
This work describes a new approach to isolate library arrays using the Biotage Quad3 FLASH system. The Quad3 system and cartridges combine to provide a major time saving technology that increases productivity in the drug discovery process. This system readily isolates and purifies 12 samples in less than 10 minutes. Typical loads for the Quad3 12M cartridge is 5 to 500 mg. With larger cartridges the Quad3 system separates up to 8 compounds in the 500 mg - 10 gram range in 10 minutes.

Download Application Note 11 (PDF - 887 kB)

Purification of a Small Combinatorial Array with C18 FLASH 12™ Cartridges
This work shows how Biotage FLASH 12M cartridges can assist chemists performing solution-phase synthesis. The refersed phase C18 packed FLASH 12 M cartridges are used as a tool to monitor the reaction progress and to isolate and identify a mixture's compounds.

Download Application Note 08 (PDF - 249 kB)

Comparative Study of Purification via Re-Crystallization & FLASH 75™
This application note compares the purification of a crude penta-peptide by conventional re-crystalization with single step purification using a Biotage FLASH 75 system. Both purification processes are easily performed on the small scale and the Biotage FLASH technique is directly scaleable to kilogram quantities.

Download Application Note 05 (PDF - 286 kB)

Trace Material Recovery by Biotage FLASH™ Chromatography
Biotage FLASH systems are powerful tools for purification of trace compounds from organic mixtures. The FLASH 12 purifications are easily scaled up to larger diameter cartridges providing recovery of gram and kilogram quantities in the same timeframe.

Download Application Note 04 (PDF - 154 kB)

Separation of Closely Related Organic Compounds via FLASH 12™
This work illustrates how adapting a flash step to isolate individual compounds in a library is very quick and easy and how Flash 12 can be used to purify a compound library.

Download Application Note 03 (PDF - 149 kB)

Purification of Protected Peptide by FLASH™ Chromatography
This paper demonstrates how the Biotage Flash 12 system provides a new powerful tool to efficiently and easily isolate the protected peptide segments resulting in high purity and good mass recovery.

Download Application Note 01 (PDF - 259 kB)