Page 7 - Shimadzu Nexera UC - Nexera UC Prep
P. 7

Analysis





 Ensures high-throughput method development and scaling up




 Automatically performs a variety of method scouting processes  Method scouting for optimization of separation conditions and scaling up
                   to preparative size
 The high-speed performance of SFC can shorten the time required for method scouting. The system automatically
 generates a large number of methods by utilizing combinations of up to 12 columns, four modifiers, and different
               For high-purity isolation,  target peaks need to be adequately separated, for which the user must determine
 ratios of modifiers to mobile phase. With the UHPLC / SFC Switching system, screening by UHPLC and SFC can be
               optimum column and separation parameter settings (method scouting). The Nexera UC chiral screening system and
 carried out in the same batch. Moreover, Method Scouting Solution, optional software for method scouting, makes it
               Method Scouting Solution can be used to screen columns more quickly and accurately (Step 1). Once the optimum
 easy to set up multiple conditions.
               column has been identified, smoothly scale up to preparative scale flow rates, preserving the peak separation
               while increasing the mass load (Step 2).
               *Preparative SFC: page 10 and following.
                Step 1   Method scouting at analytical scale

               Method  scouting is  easy even for first-time  users—simply  execute  the  batch  table generated  automatically  by Method
               Scouting Solution. The system can automatically switch between different settings to run the scouting process continuously
               day or  night, even for multiple modifiers and columns.  Various types of data can be displayed  in the data browser and
               multi-data reports generated with resolution values for all data to assist in evaluating separation conditions.
                Step 2   Scaling up                4.6 mm I.D. column (Nexera UC)
                                                   mAU (×1,000)
                                                                                 Column: Shim-pack UC-PBr 4.6 × 250 mm
               Using a Shim-pack UC series column enables you                    Flow rate: 3.0 mL/min
               to increase mass load while maintaining                           Injection volume: 20 µL
               separation performance. The optimum                               Fraction volume: 10 mg
               preparative column determined from Step 1 can
               be used to scale up the column size, flow rate
                                                   0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 min
               and injection volume based on the desired
               fraction volumes.
                                                   20 mm I.D. column (Nexera UC Prep)
                                                   mAU (×1,000)
 A screen shot of Method Scouting Solution for Nexera UC user interface.         Column: Shim-pack UC-PBr 20 × 250 mm
                                                                                 Flow rate: 56.7 mL/min
                                                                                 Injection volume: 500 µL
                                                                                 Fraction volume: 250 mg
 Chiral analysis with “Nexera UC Chiral Screening System”

 CHIRALPAK  Series and CHIRALCEL  Series columns (Daicel Corporation) for chiral analysis are capable of resolving   0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 min
 ®
 ®
 a wide variety of compounds by showing complementary separation targets. The combination of the Nexera UC
 Chiral Screening System and these columns simplifies method scouting for chiral analysis.  Selecting an SFC Column
               The HPLC mobile phase for reverse phase analysis is very different from the one used for normal phase analysis. In contrast,
               SFC uses a mixture of supercritical CO2 and a modifier (an organic solvent such as methanol) regardless of the stationary phase
 mAU
               used. Therefore, the same mobile phase composition can be used for serial analysis through all columns. Column scouting is
 300  Indapamide
 RT = 2.644    effective by using the following set of six columns, each providing a different separation selectivity.
 Rs = 2.66
 200
                                                          6 columns set
                          UC-ODS        UC-Sil II    UC-Diol II   UC-PolyVP    UC-PolyBT      UC-PBr
 100
                                                                                                   Br  Br
                                                            OH
 0                                                         OH                                    Br
                                                                                                     Br
               Chemistry                                   O                                     O  Br
 0.0  1.0  2.0  3.0  4.0  5.0  min
                                                        Si                                    Si
 Columns: CHIRALPAK  AD-3
 ®
 Modifier: Acetonitrile/Ethanol=7/3                    OH
                       The separation mode is  This is excellent for retention  The separation mode is   A favorable peak shape   This is excellent for   With ODS, separation of
                       reverse phase. Retention   of basic compounds and   normal phase. This   is obtained even   resolving aromatic   poorly retained
               Features
                        is provided through   recognition of their tertiary   inhibits non-specific   without acid-base   compounds through π-π  compounds is improved.
                       hydrophobic interaction.  structures.  interactions.  additives.  interactions.
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