Generic Compound Isolation Using Solid‐Phase Trapping as Part of the Chromatographic Purification Process. Part 1. Proof of Generic Trapping Concept.

Boughtflower, Bob; Lane, Stephen; Mutton, Ian M.; Stasica, Przemyslaw

doi:10.1002/chin.200647278

Cited by 1 publication

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“…Previous reports 3 –5 have used a fivefold aqueous dilution of fractions before or during the injection protocol to ensure that compounds are retained by the C18 column and do not break through with the solvent front.…”

Section: Resultsmentioning

confidence: 99%

“…A dramatic example is the negative impact of TFA on cultures of osteoblasts and chondrocytes even at concentrations less than 100 nM. 9 Using 19 F NMR monitoring, Boughtflower et al 3 showed the effectiveness of SPE for TFA removal from fractions eluting from HPLC columns. The advantage of TFA removal from fractions before evaporation has become a routine application of on-column solvent exchange in our laboratories.…”

Section: Removal Of Chromatographic Modifiersmentioning

confidence: 99%

“…Other authors have recently described solid-phase extraction (SPE) approaches for handling reverse-phase preparative HPLC fractions. 3 –5 In this study, the Waters (Milford, MA) on-column SPE concept 5 is adapted and customized, and the term on-column solvent exchange is used to describe the procedure of loading fractions back onto the preparative HPLC column under aqueous conditions before eluting them with acetonitrile to yield a water- and additive-free fraction.…”

Section: Introductionmentioning

confidence: 99%

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On-Column Solvent Exchange for Purified Preparative Fractions

Goetz

Beck

Tidswell

2011

JALA: Journal of the Association for Laboratory Automation

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On-column solvent exchange, using many of the principles of solid-phase extraction, has been implemented to significantly reduce evaporation cycle time following reverse-phase preparative HPLC. Additional benefits, such as a reduced potential for salt formation, thermal decomposition, and residual solvent, are also described. Fractions obtained from preparative separations, typically in a large volume of acetonitrile:water, are injected into the preparative HPLC and then eluted in acetonitrile, creating a new fraction in a volatile organic solvent. Minimal modification to the instrument was required, and unattended operation is possible. Acetonitrile evaporation is achieved within 3 h, compared with 17 h for aqueous-based fractions; lower temperatures can be used during the evaporation step; mobile-phase additives, likely to form salts with the target compound if concentrated in the fraction, are removed before evaporation; sample recovery and purity are unaffected.

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Section: Resultsmentioning

confidence: 99%

Section: Removal Of Chromatographic Modifiersmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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