UFPLC System

The Shimadzu UFPLC, Ultra Fast Preparative and Purification Liquid Chromatograph significantly reduces the cost and labor involved in preparative purification.  Additionally, the system not only performs purification of target components, but can also recover impurities with high yield enabling direct impurity analysis.

Preparative Work to Purification (Free basing Treatment) and Powderization

With conventional preparative methods, the fractionated sample contains mobile phase solvent, which leads to unavoidable dilution during fractionation, so the fractionated sample must be enriched and desalted. Such procedures complicate the workflow, and amplify sample loss, labor, and costs.

With the Shimadzu UFPLC Ultra Fast Preparative and Purification Liquid Chromatograph, all the work from preparation to enrichment, purification, and recovery is performed on-line. Using a proprietary trap enrichment purification technology for the fractionated target components, trace quantities of components contained in mixtures can be recovered at high concentrations and high purity levels. Additionally, since highly volatile organic solvents are used for the recovery of target components, the time needed for evaporation to dryness can be significantly reduced. When recovering ionic target components, counter ions are flushed out by optimization of the solution flowing through, so the target component is recovered as a high purity free base.

With these procedures, and the dedicated Purification Solution™ software, the entire process from the configuration of preparative conditions to the recovery of liquid containing the target compounds can be configured easily from simple and user friendly software.

The fully automated system can be used to purify several compounds, including the main target along with simultaneous elimination of ‘difficult-to-eliminate’ counter ions such as trifluoroacetates and low-volatility solvents which cause problems during drying or testing after purification. Whether ‘free-based’ or not, all eluted compounds are finally collected in a highly volatile organic solvent, which reduces fraction dry-down time by upto 90% compared to conventional Prep LC fractions.

• Seamless Flow from Prep LC, Trapping, Purification to Collection
• High Throughput
  • Fully Automated Workflow
  • Collection by organic solvent reducing evaporation time
• High Purity & Freebasing with TFA at target compounds less than 0.2%
• High Recovery with Unique Trapping Column
• Easy User Interface

High Speed Powderization of Cyclosporine A

The target compound fraction is repeatedly injected into the trap column, enriched by trapping, and eluted by an organic solvent. This enables recovery with a smaller volume of liquid, so subsequent powderization can be performed in a shorter time. In this way, the same volume of powdered sample can be purified in a shorter time versus elution in reverse phase conditions.

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Fraction of                             Fraction                          Fraction                            Drying

Cyclosporin A                        vol.(mL)                       conc.(mg/mL)                 time* (min)

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    Prep LC                              62.5                                        0.04                           290

    UFPLC                                8.10                                        0.29                             70

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Comparison of Preparative LC and UFPLC Fractionation

• Comparison of drying times when a centrifugation enrichment dryer is used