Automatization for development of HPLC methods

Within the frame of inprocess analytics of the synthesis of pharmaceutical drugs a lot of HPLC methods are required for checking the quality of interm ediates and drug substances. The methods have to be developed in terms of o ptimal selectivity and low limit of detection, minimum running time and chr omatographic robustness. The goal was to shorten the method development pro cess. Therefore, the screening of stationary phases was automated by means of switching modules equipped with 12 HPLC columns. Mobile phase and temper ature could be optimized by using Drylab((R)) after evaluating chromatogram s of gradient elutions performed automatically. The column switching module was applied for more than three dozens of substances, e.g. steroidal inter mediates. Resolution (especially of isomeres), peak shape and number of pea ks turned out to be the criteria for selection of the appropriate stationar y phase. On the basis of the "best" column the composition of the "best" el uent was usually defined rapidly and with less effort. This approach leads to savings in manpower by more than one third. Overnight, impurity profiles of the intermediates were obtained yielding robust HPLC methods with high selectivity and minimized elution time.