October 27, 2014 – BrightSpec will present two posters at the 2014 Eastern Analytical Symposium from November 17-19 in Somerset, NJ. We encourage you to come out, visit us at the booth or posters and learn about the instruments and techniques that BrightSpec offers.
Pharmaceutical residual solvent analysis using Fourier Transform Molecular Rotational Resonance (FT-MRR) Spectroscopy
Brent J. Harris, BrightSpec, 770 Harris St., Ste. 104B, Charlottesville, VA 22911, Robin L. Pulliam, Roger Reynolds, Justin L. Neill, Matthew T. Muckle, Brooks H. Pate
Residual solvent content is a critical quality attribute (CQA) in pharmaceutical manufacturing that has motivated the search for new process analytical technology (PAT). The standard gas chromatography (GC) methods require hours of calibration and suitability testing that are incompatible with process monitoring applications. Fourier transform molecular rotational resonance (FT-MRR) offers a powerful alternative for fast, direct analysis of volatiles (including water) in pharmaceutical drug development and process monitoring applications. A single analyte can be detected at 100 ppm (m/m) levels in as few as 10 seconds. The technology platform is inherently selective and adaptable to enable monitoring of an extensive list of volatiles without chromatography or chemometrics. Detection targets can be re-assigned arbitrarily by selecting pre-defined measurement protocols that include a double resonance analysis for unambiguous identification of analytes in the mixture. FT-MRR performance for residual solvent analysis is presented using the headspace of a custom mixture with a GC verified composition of common solvents dissolved in water and dimethylacetamide (DMAC). The results summary includes cycle time, detection limits, linearity, and reproducibility. The broader implications include applications of FT-MRR to in-line batch drying analysis, high throughput residual solvent analysis, genotoxic impurity analysis, and chiral analysis.
New techniques for the analysis of volatiles and gases: Fourier Transform Molecular Rotational Resonance (FT-MRR) Spectroscopy
Justin, L. Neill, BrightSpec, 770 Harris St., Ste. 104B, Charlottesville, VA 22911, Robin L. Pulliam, Roger Reynolds, Brent J. Harris, Matthew T. Muckle, Brooks H. Pate
For gas mixture analysis, there is a need for new instruments that offer standalone operation in combination with broad composition analysis capabilities. Infrared based detectors come with constraints in selectivity and chemical coverage, and gas chromatography techniques come with the need for a dedicated analyst. A new commercial molecular spectroscopy technique, FT-MRR, is capable of direct, quantitative gas mixture analysis without chromatography. The FT-MRR spectral fingerprint is specific to the unique mass distribution of a molecule (including its isotopes) and arises from the quantized rotational energy levels. It is also a high resolution technique that offers superior chemical selectivity over infrared spectroscopy for complex mixture analysis. Without the need for optical cavities, a broadband FT-MRR instrument can monitor a wide range of volatile species, and is reprogrammable in order to incorporate new compounds. The detection limits for small, polar molecules (e.g. HCN, NH3, H2S, H2CO, H2O) in direct sampling are in the parts-per-billion (ppb), with parts-per-trillion (ppt) attainable with a pre-concentration sampling system. FT-MRR performance for quantitative analysis using calibration standards in nitrogen will be presented. Sampling methods for direct analysis as well as pre-concentration for trace monitoring of volatile organic compounds in air will be described.