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On-line HPLC combined with multivariate statistical process control for the monitoring of reactions |
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| Authors: | Zhu Lifeng Brereton Richard G Thompson Duncan R Hopkins Paul L Escott Richard E A |
| Affiliation: | a Centre for Chemometrics, School of Chemistry, University of Bristol, Cantocks Close, Bristol BS8 1TS, UK b Glaxo Smith Kline, GlaxoSmithKline, Gunnels Wood Road, Stevenage, Hertfordshire SG1 2NY, UK c GlaxoSmithKline, Old Powder Mills, Tonbridge, Kent TN11 9AN, UK |
| Abstract: | On-line high performance liquid chromatography is used to monitor a steady state reaction over 35.2 h, with 197 chromatograms recorded as the reaction progresses. For each chromatogram, peaks are detected, baseline corrected, aligned and integrated to provide a peak table consisting of the intensities of 19 peaks, two corresponding to the reactants, one to the product and one to the solvent, the remaining being impurities, by-products or intermediates. D-charts and Q-charts from multivariate statistical process control are applied to the data to determine which samples are out of control and also provide diagnostic insight into why these samples are problematic. The D-chart is best at looking at overall performance issues such as problems with mixing or difficulties with instrument operation, whereas the Q-charts are best at detecting impurities during the reaction. |
| Keywords: | On-line high performance liquid chromatography (HPLC) Process monitoring Chromatography Multivariate statistical process control (MSPC) |
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