PITTCON 2008

March 3–6, 2008

Ernest N. Morial Convention Center
New Orleans, LA, USA

Conference Details

Booth #5456

Poster Schedule

Talk Schedule

Monday, March 3, 2008
Time: 11:05 AM (Slot #9)
Location: Room 349
Abstract #: 450–8

SESSION: HPLC: Pharmaceutical Applications
TITLE: Efficient Development of Chiral Chromatographic Methods
Teresa Ponzio and Michael McBrien (ACD/Labs)

Abstract: The development of separations for enantiomers remains a considerable challenge in the world of biologically-relevant chemistry. Chromatographers must develop methods for separations on both the analytical and preparative scale. A complication in this process is the fact that it can be quite challenging to predict the system of choice for a given molecule. On the other hand, once a system has been found that shows selectivity between the molecules of interest, optimization is a relatively facile process. Chromatographers have generally taken the approach of screening a considerable number of orthogonal systems to locate an optimizable system for separation. Many injections are performed, and the chromatograms are reviewed to locate the system that is most favorable for optimization. Typical review systems, however, can be inefficient. The onus is on the chromatographer to manually review each chromatogram, sometimes amounting to hundreds of datafiles per day. This process is of course time-consuming. Equally disappointing, typically all of the results of the screens, positive and negative, are discarded. The loss of this considerable knowledge is especially disappointing in light of the fact that many of these molecules will remain active in the organization for some time after the separation is developed. There is an excellent chance that screens will have to be performed again at a later point in the life of the molecule. Recently, systems have been designed to increase the efficiency of chiral screening, while preserving the knowledge gained for retrieval within the organization. These systems work through the connection of multiple data systems, automatically linking sample data with chromatographic and structural information, and providing a streamlined interface for chromatogram review. All of the selectivities measured are automatically stored within a searchable knowledgebase.

Monday, March 3, 2008
Time: 1:30 PM (Slot #1)
Location: Room 269
Abstract #: 760–1

SESSION: Liquid Chromatography/Mass Spectroscopy: Software and General Applications
TITLE: Chromatographic Method Development: An Approach Incorporating UPLC, MS and Modeling Software to Streamline the Process of Creating Robust Methods
Lauren Wood (Waters) and Michael McBrien (ACD/Labs)

Abstract: This study demonstrates the utility of Ultra Performance Liquid Chromatography (UPLC) technology, single quadrupole MS and chromatographic modeling software to facilitate an efficient method development process of impurity profiles for pharmaceutical drug entities. The HPLC method for Simvastatin has been redeveloped on UPLC to be compatible for MS. The analytical goals were to meet the requirements stated in the USP 30 - NF 25 monograph for the Simvastatin drug substance and drug product chromatographic purity and assay identification. Chromatographic modeling software was used to aid in the iterative method development decision-making process by systematically assessing method parameters such as stationary phase, solvent, temperature, pH, gradient, and mobile phase additives during both the screening and optimization steps of method development. This software was also used to automatically program the predicted instrument conditions in the chromatography data system (CDS) software, thus automating instrument control. UV and MS Peak Matching routines were used to identify and match peaks between injections and datasets based on spectral similarity between components. User-defined mathematical calculations and specialized reports were also used in streamlining the decision-making process during method development. The use of UPLC in combination with single quadrupole MS with electrospray positive/negative ionization detection aids in the discovery of any impurities which contain no chromaphores. Pre-validation of the methodology to verify specificity, linearity, accuracy, and precision was also performed for verification of method conversion equivalency.

Tuesday, March 4, 2008
Time: 10:25 AM (Slot #7)
Location: Room 274
Abstract #: 1140–6

SESSION: Lab Informatics I
TITLE: Focusing on the Analytes in Complicated Mixtures by Componentization and Filtering of LC/MS Data
Graham A. McGibbon (ACD/Labs)

Abstract: Saving analysts’ time and effort are key advantages that advanced software algorithms can provide when identifying drug molecules, therapeutic and illicit, and their metabolites in complicated mixtures, which is still a real challenge despite the use of sophisticated instrumentation. Compound recognition by software relies on the auto-componentization, fragment extraction and peak-tagging of MS data. Many metabolite profiling experiments for drug development rely on the use of radiolabeled compounds for mass balance and products finding, so different types of chromatographic data must be viewed together. We have recently developed a prototype filter for non-natural isotope abundances that can be applied to find radiolabeled metabolites in datasets generated from these types of samples. One example is for a sample containing 14C-Buspirone. The use of the novel isotope filter with appropriate 13C:14C ratios provided a short list of priority components, including expected and unexpected metabolites with only one false positive result after the application of the filter. All metabolites known to be present in this dataset were extracted by the Isotope Ratio Filter, without the use of the control sample as a comparison. The Isotope Ratio Filter is not only useful for radiolabeled samples; it is also useful for extracting chlorinated, brominated, or sulfinated compounds based on their characteristic isotope patterns. The componentization algorithm can advantageously process accurate mass or low resolution data and can be used for targeted screening investigations of complicated samples including biofluids.

Wednesday, March 5, 2008
Time: 10:05 AM (Slot #6)
Location: Room 269
Abstract #: 1860–5

SESSION: Characterization of Polymers and Plastics I
TITLE: Interpreted IR and Raman Databases
Michael Boruta (ACD/Labs), Gene S. Hall, Ph.D (Rutgers University), Michel Hachey (ACD/Labs)

Abstract: When searching IR or Raman spectra against spectral databases, not finding an exact match is more common than we would like. This is less frequent than one would expect with over 10,000,000 compounds in the world and some 100s of thousands of reference spectra. However, just because an exact match is not found does not mean that the search did not provide us with helpful information. Often there is useful information about the classification of the unknown and some guidance in the interpretation of the unknown material. The difficulty is in extracting that information from the reference database. Having a database that includes spectral structure correlations can make that task easier. This talk will report on an ongoing project to develop interpreted IR and Raman databases to assist in the identification, interpretation, and classification of results from spectra searching.

Wednesday, March 5, 2008
Time: 11:05 AM (Slot #9)
Location: Room 274
Abstract #: 1890–8

SESSION: Lab Informatics II
TITLE: Achieving Great Science Bringing Together Physical Measurements and Chemical Analysis
Michael Boruta (ACD/Labs), Michel Hachey (ACD/Labs), Keith Kociba (B&K Publishing)

Abstract: In today’s laboratory it is common to be involved in many aspects of the physical/chemical analysis of materials. Having the ability to keep track of all of this disparate data can be a major challenge, whether we are generating all of the data ourselves or it is coming from several departments. In addition, with all of this different data the possibility of misplacing something is much higher than we would like to admit. This talk will look at a tool that can be used to manage, analyze, annotate, and create reports from data sources as diverse as TGA, DSC, XRPD, optical spectroscopy, chromatography, Mass Spec, NMR, chemical structures, and meta-data. Having all of the data available to review and share across an organization improves the decision-making process and allows great science to be achieved.

Thursday, March 6, 2008
Time: 10:25 AM (Slot #7)
Location: Room 274
Abstract #: 2530–6

SESSION: Chemometrics
TITLE: Robustness of Variable Selection Based on Pure Variables
Michael Boruta and Michel Hachey (ACD/Labs)

Abstract: Since many wavelength selection methods can produce wildly different wavelength suggestions providing small changes in the data set, it is interesting to examine how robust the recently proposed pure variable method for selecting wavelength is. In this method, the variable selection method is guided by the purity function from the SIMPLe-to-use Interactive Self-modeling Mixture Analysis (SIMPLISMA) algorithm to help determine the most significant and influential regions in a multivariate calibration. A series of publicly available data sets will be used to study the robustness and help differentiate this method from alternate wavelength selection strategies that are more statistically focused.

Poster Schedule

Tuesday, March 4, 2008
Time: Slot #11
Abstract #: 1240–11

SESSION: Liquid Chromatography/Mass Spectrometry: Pharmaceutical Applications
TITLE: Strategies for Automated Chromatographic Method Development
Teresa Ponzio and Michael McBrien

Abstract: Automated chromatographic method development has recently become a topic of considerable interest to the analytical chemistry world. The design of effective chromatographic methods is a complex task involving the often conflicting goals of separation robustness, resolution of all components of interest, and fast run time. The chromatographer has an unprecedented array of tools available for this difficult task, including ultrahigh performance liquid chromatography, mass spectrometry, unique new mobile phase selectivities, chemometric component detection and tracking, automated decision-making, and workflow and project management software. While the method development toolset has advanced considerably over the last few years, method development strategies have remained fairly stagnant. This paper will present new strategies for chromatographic method development that leverage these modern method development tools, resulting in increases in method development efficiency. The strategies shown are designed to increase the effectiveness and rigor of method development, while decreasing the amount of time that users are required to manually review method development data. A combination of screening and optimization method development “waves” maximize the selectivity space investigated without sacrificing effectiveness of chemometric peak tracking. Instrument control is leveraged to minimize the time required configuring injection sequences. The approaches will be illustrated with several real-world examples.

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