Page 14 - Clinical-MedicalSolution for Medical Chemistry

UFPLC

Ultra Fast Preparative and Purification LC System

When developing new drugs, structural analysis of impurities and metabolites is a critical process. Puri cation solution simpli es settings related to preparative puri cation
Analyzing the structure of target components in the fractionated liquids obtained after puri cation of
The special Puri cation Solution software is equipped with peak tracking functions that enable the target peaks and fractionate
synthesized substances using a preparative LC system is time-consuming. In addition, it is dif cult to
and be checked at a glance.
recover target components with high purity.
However, using the UFPLC system, all preparative processes can be performed online, from Chromatogram
fractionation to concentration, puri cation, and recovery, which can signi cantly reduce the time Individual fraction peaks are color-coded.
required for preparative puri cation. In addition, using Shimadzu's unique trap concentration and Trap Column
puri cation technology, trace components included in synthesized substances can be recovered at high Trap columns are displayed with the same color as their corresponding
concentrations and with high purity. Due to the high volatility of the organic solvents used to recover faction peaks.
target components, the solvents can be evaporated and components dried in less than one tenth the time Fraction Collector
of previous systems. This displays which vial in the fraction collector was used to collect the
Furthermore, using a rinse solution to rinse away counter ions means target components can be eluate recovered from the trap column.
recovered as a high-purity free base. Consequently, it signi cantly improves the quality of new drug Elution Chromatogram
discovery research, such as for ef cacy screening and pharmacokinetic testing for drug candidates The chromatogram range is color-coded in accordance with the trap
affected by counter ions. column and fraction collector vial display colors.

Isolates fraction containing
target peaks and concentrates Applications
it in a trap column

Removal of salts in the mobile phase solvent 400 mAu
Removes impurities and Trapping column 1 Prep LC
pair ions Removal of ammonium Trapping column 2 Valerophenone
chloroacetate salts from ibuprofen 300 Trapping column 3
Target
compounds Elutes components using Ibuprofen, the target component, is cleaned by retention in a 200 Ammonium
organic solvent trap column. As a result, the ammonium chloroacetate salts 100 Ibuprofen Chloroacetate Salts
Fractionation/
Pair ion concentration contained in the mobile phase solvent were removed. This can 0 UFPLC
(ex TFA) prevent the retention of salts contained in the mobile phase 0.0 2.5 5.0 7.5 min
solvent during powderization, so that only the target Preparative Chromatogram for
Sample containing Puri cation Ibuprofen and Analogous Substances (UFPLC)
target components component is recovered. Ibuprofen
Heightening the ef ciency of enrichment puri cation for trace components
High speed powderization of cyclosporine A
Elution
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 puri ed in a shorter time versus elution in reverse phase conditions.

Recovery of target Comparison of Preparative LC and UFPLC Fractionation 15 minutes
×
compounds in 5 cycles 290 minutes
Typical
high-purity liquid Fraction of Fraction vol. Fraction conc. Drying time* Preparative Preparative Total:
Cyclospolin A (mL) (mg/mL) (min) Work Powderization
LC 365 minutes
Prep LC 62.5 0.04 290
UFPLC 8.10 0.29 70 UFPLC Preparative Enrichment Powderization Total: 160 minutes
Work Purification
* Comparison of drying times when a centrifugation enrichment dryer is used 15 minutes 15 minutes 70 minutes
×
5 cycles
Comparison of Procedural Times for Typical Preparative LC and UFPLC
Solutions for Medicinal Chemistry
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