RESUMO
Following purification, the fractions of purified samples typically are analyzed to determine the relative purities of each fraction. We report a novel technique for performing post-purification analysis immediately after each preparative LC/MS run. The Single Pass Compound Purification and Analysis System (SPACPASS) samples and stores a representative aliquot from the fraction while it is being collected. Demonstrated for '1:1' fraction collections, this method of fraction purity assessment streamlined sample processing by reducing post-purification sample handling. For 97% of the collected fractions, this technique provided relative purities to within +/-5% when compared with more traditional post-purification analysis.
Assuntos
Cromatografia Líquida/métodos , Calibragem , Espectrofotometria UltravioletaRESUMO
In this paper we report using a parallel, four-channel HPLC/MUX/MS purification system, the Purification Factory, to purify thousands of compounds destined for high-throughput screening in a single month. The maximum sample throughput during this 20-workday month was 704 samples/day. Since this purification throughput exceeded the postpurification sample and data handling capabilities provided by commercial solutions, a custom-integrated solution was designed to address these shortcomings. In this paper we detail the key improvements in automation, solvent handling, and sample handling logistics implemented to sustain a mean throughput of 528 samples/day over a multimonth time period.