May 01, 2015 - Columbia, MD
Sampling chemical reactions for offline analysis by HPLC, NMR and other analytical techniques to determine reaction progress, yield or impurity profiles is a well-established practice. Unfortunately, the sampling process is not always a precise operation and presents significant challenges for reactions with heterogeneous mixtures, elevated temperatures, slurries, or involving air sensitive chemistry. Furthermore, delays in quenching can lead to highly variable results and inaccurate and imprecise analytical information. EasySampler was designed to eliminate these challenges by providing an automated and robust inline method of taking representative samples from reactions, even in difficult conditions. At Pfizer and other pharmaceutical companies, scientists have been applying EasySampler to support their synthetic chemistry and process development activities.
With the adoption of robust, automated lab reactors, chemists are able to run their experiments overnight or when away from the lab. But, there has been no good way to robustly and representatively sample, and collect critical information concerning yield and reaction completion. While the integrated use of in situ PAT tools, such as Fourier Transform Infrared (FTIR) Spectroscopy and Raman, can provide a comprehensive analysis of the reaction in real time, critical information concerning impurity profiles are typically not easily obtained or may not be available. Offline techniques such as HPLC, UPLC, and GC are considered to be the standards for these analyses, but even they require a sampling system to ensure high quality representative measurement over the timeframe of the entire reaction. EasySampler provides unattended, automated chemical reaction sampling, allowing chemists to run experiments and gather data while at home or in meetings; thus significantly increasing their productivity.
The unique patented EasySampler probe enables the capture and immediate quenching of reaction samples in the reaction vessel, in real time, ensuring that samples are truly representative of their reactions at the time of sampling. Capturing a representative sample is especially important when dealing with low temperature or air sensitive reactions.
EasySampler ensures samples are captured and quenched at actual reaction conditions eliminating any environmental influence such as exposure to increased temperature or oxygen. By fully automating the sampling process 24 hours a day, manual sample handling is eliminated. This reduces risks and improves operator safety, especially when dealing with highly toxic chemistry.
Chemists in the pharmaceutical and chemical industries have applied EasySampler over a wide range of chemistries and conditions. For instance, EasySampler has been used in long term stability studies over several days and in reactions which require immediate quench-in-place operation at reaction temperatures. Samples have been applied for kinetics studies with modeling quality data. Reaction types that have been successfully studied include:
Thick Slurries
Viscous Reactions
Undissolved Inorganics
Tri-Phasic Mixtures
Ullman Reactions
Oxygen-Sensitive Reactions
EasySampler provides a unique method of capturing, quenching, and preparing each sample.
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