Препаративная ВЭЖХ система на базе блоков LC-40 Nexera

  • Описание
  • Conditions
  • Nexera Prep
  • Separation
  • Expandability
  • Options

Описание

  • Easy optimization of preparative parameters and scale up
  • Fractionation simulation for rapid setup of collection logic Column line-up for scale-up from analytical to preparative
  • Time- and energy-saving by automation of the purification workflow
  • Collection of target components at high purity by automated desalting
  • Expandable to suit the sample/fraction number and volume
  • Choose from a wide range of options for recovery scale and analytical detection Problems are resolved simply, to accommodate a variety of needs.

Streamline and Simplify Establishing
the Conditions for Preparative Work
Using the Nexera™ Prep system saves on labor when scaling up from the development of analytical conditions to the conditions for preparative work.

Preparative Work for Target Components at High Purity Levels and High Concentrations
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 for Target Components at High Purity Levels and High Concentrations
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 for Non-UV Absorptive Components
With LH-40 and FRC-40 able to perform signal-based logic and collection on up to four signal channels, not having a chromophore is not a limitation. Nexera Prep can use LCMS, RID, and ELSD to detect and/or identify targets for purification.

High Separation via Preparative Recycling
By repeatedly cycling the sample through the column, the target component can be resolved and recovered from coeluting species or impurities without the need for longer or multiple columns.

Excellent System Expandability
The solvent delivery unit and fraction collector can be selected to suit the recovery volume.
Additionally, the Shim-pack™ Scepter features excellent scalability from analysis to preparative work, and the preparation of a variety of components is supported by an ample lineup.

Conditions

Streamline development of Analysis Conditions and Optimization of Preparative Parameters

In order to separate multiple components, the analysis and fractionation parameters must be optimized, which involves a great deal of work.
Shimadzu provides the Method Scouting system, which investigates conditions at the analytical level. Method Scouting system fully automates method scouting in which combinations of mobile phases and columns are automatically changed, equilibrated, and evaluated, allowing efficient method development.
Further, the preparative system performs automatic simulations using the pre-preparative results, enabling optimization of the fractionation parameters.
This reduces the work involved in investigating conditions, which saves on mobile phase solvent and samples.

Development of Analytical Conditions (Method Scouting System)
A development is performed to separate the target compounds at the analysis level.
Using the Shimadzu Method Scouting system together with Method Scouting Solution, a special software program, provides a fast and accurate method scouting workflow, which supports heightened efficiency in method development.

Significantly Reduces the Process of Setting Fractionation Parameters

Simple parameter setting by fraction simulator

LabSolutions™ software provides simulation functions that reduce the labor involved in investigating conditions for analytical and preparative work.
With the LabSolutions fractionation simulator (patent pending), specify the peak segment in the chromatogram to fractionate, and the system automatically sets the parameters required for fractionation. This reduces the time spent on setting fractionation conditions to about 1/4 the typical expenditure.

Noise skipping by new algorithm

When configuring fractionation via automatic peak recognition, noise in the chromatogram is sometimes mistaken for component peaks, resulting in an insufficient number of test tubes for intended collection or improper positioning of collected fractions. With the LabSolutions software Peak Sensitivity Determination function (patent pending), peaks are recognized from the number of data points consecutively exceeding the configured threshold value, to determine whether to fractionate.

 

Fraction Purity Checks(LH-40)

A fraction purity check can easily be performed with a single system. Purity checks can be performed without changing the fraction recovery container, so the workload is reduced and throughput is improved.

 

Sample rescue function prevents the loss of precious samples(LH-40, FRC-40)

Even if a problem occurs during preparative work, the sample remaining in the system can be recovered. By following the rescue instructions, the precious sample is recovered into the specified container rather than being discarded. Additionally, by using the optional waste collector, samples that cannot be recovered due to fractionation mistakes can be retained.

Nexera Prep

Preparative system general HPLC: Nexera Prep

Significantly Reduces the Processes Involved from 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. This significantly reduces the labor involved in the preparative purification process, and avoids procedural mistakes. 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.

Automation of the Preparative Purification Process
When target compounds are to be powderized, this process can be hindered by a number of factors including the presence of acids, salts, and refractory solvents. With the UFPLC Ultra Fast Preparative and Purification Liquid Chromatograph, these hindrances to powderization can be removed by flushing them out using a trap column, allowing a high purity powder of the target component to easily be obtained by anyone.

Even Trace Components Are Recovered at High Concentrations
Normally, when preparing trace quantity target components, preparative work involves injecting the sample multiple times to obtain sufficient amounts of the target. As a result, the volume of fractionation liquid ultimately obtained increases in proportion to the number of injections, increasing solvent use and dry down time. With the UFPLC Ultra Fast Preparative and Purification Liquid Chromatograph, even with multiple injections, the fraction of the target component is injected into the same trap column for enrichment. The final volume of fractionated liquid from the trap column is minimized, exchanging the weaker loading solvent for a suitable organic solvent. The target component can then be recovered at high purity levels and at high concentrations.

Purification Solution Simplifies Settings Related to Preparative Purification
The special Purification Solution software is equipped with peak tracking functions that enable the target peaks and fractionate and be checked at a glance.

Applications
Removal of Salts in the Mobile Phase Solvent

Removal of Ammonium Chloroacetate Salts from Ibuprofen
Ibuprofen, the target component, is cleaned by retention in a trap column. As a result, the ammonium chloroacetate salts contained in the mobile phase solvent were removed. This can prevent the retention of salts contained in the mobile phase solvent during powderization, so that only the target component is recovered.

Heightening the Efficiency of Enrichment Purification for Trace Components
High Speed Powderization of Cyclosporine A
The target compound fraction is repeatedly injected into the trap Ibuprofen 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.

Preparative system general HPLC: Nexera Prep

Using MS Signal Triggers Enables Recovery with no Target Fraction Omissions
It can be difficult to prepare low UV absorptive components using just a UV signal as the trigger, so there is a risk that the fraction will be missed.
By using the MS signal as the trigger, the preparative work can be performed simply, with nothing missed. By specifying the m/z of the target component, fractions can be collected with confidence. The LCMS-2020 mass spectrometer enables high-sensitivity and high-resolution detection for preparative work with no target components omitted.

High Purity Recovery of Target Components Using Multiple Signal Triggers
By combining up to four detector signal channels, target components can be recovered at high purity levels.
The MS signal from the detection of target component A is used as the trigger to start fraction collection. The MS signal from the detection of impurity B, which is eluted in proximity, is used as the trigger to stop fraction By combining multiple triggers in this way, it is possible to recover only the target component at high purity level. Combining a variety of detector signals as triggers, targets can be recovered at high purity levels, with the confidence that all peaks were detected.

The MS signal from the detection of target component A is used as the trigger to start fraction collection. The MS signal from the detection of impurity B, which is eluted in proximity, is used as the trigger to stop fraction By combining multiple triggers in this way, it is possible to recover only the target component at high purity level. Combining a variety of detector signals as triggers, targets can be recovered at high purity levels, with the confidence that all peaks were detected.

Optional Analytical and Preparative Open Solution™ Software Simplifies
Preparative Operations and Data Analysis
Efficient System Sharing via Open Access
Open Solution simplifies the sharing of preparative systems between several people.

There is a special sample registration window, so preparative work can be performed easily just by having users log in and then specify their method, injection volume and target m/z.

Preparative Operations and Data Analysis can be Performed from a Single Window
With the Open Solution data browser, preparative results can be checked from a single window.
When the test tubes are selected, the peaks are highlighted, and the MS spectrum and UV spectrum for the applicable peak are displayed.
The information for the fractionated compound can be checked easily.

Separation

High Separation via Preparative Recycling

What is the recycling separation method?
Long preparative columns are expensive, as such there is a need to use comparatively lower cost short columns effectively.
In the recycling separation method (closed valve recycling), the eluate liquid containing the target components that has eluted from the separation column is recycled into the column, enabling an equivalent separation capacity to that of a longer column.

Recycle-Assist — Special Preparative Recycling Software*
Perform Automatic Preparative Recycling with a Simple GUI-Based Operating Environment
The graphical user interface (GUI) provides an environment where even novices to preparative recycling can perform operations simply and reliably. A single main window is used for the workflow from recycling to fractionation, thus reducing the risk of wasting precious samples through setting mistakes.

Recycling Conditions are Completely Set in Three Steps
Just click three points corresponding to the recycling start, recycling stop, and automatic collection start point to complete the settings for the recycling preparation conditions. Entering complicated numerical parameters is completely unnecessary, so recycling preparative work can start easily.

Expandability

Excellent System Expandability

Solvent Delivery Unit Accommodates a Wide Range of Recovery Volumes
Guidelines for Preparative Scale and Maximum Load

The figure at right shows the guidelines for total component capacity with a 250 mm long column when the target component is highly soluble in the mobile phase, separates from impurities, and ions are suppressed. For isocratic elution, in principle, the total component capacity is proportional to the column volume.

Guidelines for Preparative Scale and Maximum Load

  • LC-20AT
    This solvent delivery unit can handle flow rates ranging from those used in analytical scale to those used in semi-preparative (up to 10 mL/min).
    High-precision analysis is possible even in the semi-micro flow-rate range.

Supports Semi-Preparative and Recycle Preparative

  • LC-20AR
    This solvent delivery unit can handle flow rates used in semi-preparative scale (up to 20 mL/min).
    Using a recycle kit enables semi-preparative recycling.

Supports Large-Scale Preparative Fractionation

  • LC-20AP
    High flow rates (up to 150 mL/min) enable highly efficient, large-scale preparative fractionation.
    Large-scale prep solvent delivery fully supports the preparative fractionation workflow including reinjection to assess purity.
    Combine with an FCV-200AL low-pressure gradient unit to perform gradient analysis using up to four mobile phases.
LC-20AT LC-20AR LC-20AP
Solvent delivery method Series-type double plunger Parallel-type double plunger
Plunger capacity Primary side: 47 μL, Secondary side: 23 μL 47 μL 250 μL
Maximum discharge pressure 40 MPa 49 MPa 42 MPa
Flow rate setting range 0.001 to 10.000 mL/min 0.001 to 20.000 mL/min 0.01 to 150.00 mL/min
Flow rate accuracy
No more than ±2% or ±2 μL/min,
whichever is greater (0.01 to 5 mL/min)
No more than ±1% or ±10 μL/min,
whichever is greater (0.1 to 5.0 mL/min)
No more than ±1% (1 mL/min, 10 MPa)
Flow rate precision No more than 0.06% RSD or 0.02 min SD,
whichever is greate
No more than 0.08% RSD or 0.02 min SD, whichever is greater No more than 0.1% RSD or 0.02 min SD,
whichever is greater
Constant pressure solvent delivery Supported
Plunger rinsing mechanism Syringe or rinsing pump Syringe or rinsing pump
Operating temperature range 4 to 35 °C 4 to 35 °C 4 to 35 °C
Size and weight W 260 x H140 x D 420 mm,11 kg W 260 x H140 x D 500 mm,16 kg W 260 x H210 x D 500 mm,19 kg

Shim-pack Scepter Columns
— Excellent stability & performance using a wide range of LC conditions —
Shim-pack Scepter LC columns, which are the next generation organic silica hybrid based columns, are designed for stability and performance in a wide range of mobile phase conditions. With different chemistry characteristics, Shim-pack Scepter columns are effective for method development/scouting under conditions that may compromise traditional silica based columns.
With different particle sizes (1.9 μm, 3 μm, 5 μm) and different column dimensions, Shim-pack Scepter LC columns are fully scalable between UHPLC, HPLC and preparative LC, making method transfer seamless between different laboratory instrumentation.

Shim-pack Scepter Reversed Phase
C18 HD-C18 C8 Phenyl PFPP
Functional Group Trifunctional C18 Trifunctional C18 Trifunctional C8 Trifunctional
Phenylbutyl
Trifunctional
Pentafluorophenylpropyl
Generic Purpose Type High Density Type
Particle Organic Silica Hybrid
Particle Size 1.9 μm,3 μm,5 μm
Pore Size 12 nm 8 nm 12 nm
End Capping Proprietary None
pH Range 1 — 12 1 — 10 1 — 8
100% Aqueous Condition Yes No No Yes Yes
USP Classification L1 L1 L7 L11 L43

The LH-40 Liquid Handler, Combination of Autosampler and Fraction Collector
Options
Syringe Kit 20 mL
This kit enables large-capacity injections of 2 mL or more at one time. The maximum injection volume is 20 mL.

Washing Pump
This reduces the washing time for the injection needle, increasing throughput while reducing carryover.

Analysis Kit
The recovered fraction can be reanalyzed to check the purity.

Liquid Surface Detection Needle
This detects the liquid surface level, and automatically determines whether there is any sample present. As a result, only the remaining volume is injected, which prevents the injection of air into columns. Additionally, if no sample is present, the system can proceed to the next sample, reducing needless errors and lost labor.

Autosampler
SIL-10AP
Sample Racks
・Sample rack S for 1.5 mL vials
・Sample rack L for 4.0 mL vials
・Sample rack LL for 13 mL vials*1
*1 Sample rack LL is a standard accessory of the SIL-10AP

Sample Coolers
Block Cooling/Heating: 4 to 70 °C)

Manual Injecto
Rheodyne®7725
Optional Sample Loops (Material: SUS)

Specifications

LH-40 SIL-10AP
Maximum Number of Containers Up to 540 pcs* (10 mm I.D. test tubes) Up to 100 pcs* (1.5 mL vials)
Maximum Injection Volume Up to 20 mL (with the Large Capacity Injection Kit) Up to 5 mL
Cooling Function None Yes (Optionally available)
Compatible Containers and Quantities
10 mmO.D. test tube 540 pcs
12 mmO.D. test tube 486 pcs
16 mmO.D. test tube 216 pcs
18 mmO.D. test tube 216 pcs
25 mmO.D. test tube 108 pcs
35 mmO.D. test tube 54 pcs
MTP/DWP 9 pcs
1.5 mL vials 100 pcs
4.0 mL vials 80 pcs
13 mL vials 25 pcs
Compatible Containers and Quantities W 390 x H 560 x D 730 mm, 40 kg W 260 x H 280 x D 320 mm, 18.5 kg

* Depends on the type of racks used

FRC-40, Highly Flexible Fraction Collector
Sample Racks

A variety of containers can be placed including MTPs, vials, and various types of test tubes. Six colors are available, so a separate color can be apportioned to each user in order to avoid confusing samples.

Multi Fraction Collector Kit
Up to six FRC-40 fraction collectors (up to five LH-40 liquid handlers) can be connected, making it easy to increase the number of fractions.

Compact Design for Small-Volume Samples
FRC-10A
For smaller scale collection, or specialized applications that require enclosure and cooling, the FRC-10A is a compact fraction collector that provides time and signal based triggering. A variety of programmable fractionation functions enable target components to be collected with high purity and high recovery.。

Specifications

FRC-40 FRC-10A
Maximum Number of Fractions Up to 540 pcs* Up to 144 pcs*
Maximum Flow Rate 150 mL/min
Fractionation Mode Configured through a combination of basic mode (initial parameter mode) and time program mode (14 parameters)
Cooling Function None Optionally available
Compatible Containers and
Quantities
10 mmO.D. test tube   540 pcs 4 mL vial 252 pcs
12 mmO.D. test tube 486 pcs 15 mL vial 108 pcs
16 mmO.D. test tube 216 pcs 50 mL vial 54 pcs
18 mmO.D. test tube 216 pcs 250 mL vial 20 pcs
25 mmO.D. test tube 108 pcs 500/1000 mL bottle 12 pcs
35 mmO.D. test tube 54 pcs MTP/DWP 9 pcs
10 mmO.D. test tubes 144 pcs
18 mmO.D. test tubes 164 pcs
35 mmO.D. test tubes 16 pcs
Size and weight W390 × H560 × D730 mm, 30 kg W 260 x H 280 x D 420 mm,15 kg
* Depends on the type of racks used.

Options

Column Hub
Column Holder
Column Holder, SLIM
Preparative columns with an I.D. of 20 mm to 50 mm as well as manual switching valves can be attached. The valves can be used for column switching.

Specifications

Installable Valves Installable Columns Size
Column Hub Automatic Switching Valves Up to 4 pcs Preparative Columns 2 pcs Analytical Columns 6 pcs* W 260 x H 560 x D 500 mm
Column Holder Manual Switching Valves Up to 4 pcs Preparative Columns 2 pcs Analytical Columns 1 pc W 250 x H 465 x D 400 mm
Column Holder SLIM Manual Switching Valves Up to 5 pcs Preparative Columns 2 pcs Analytical Columns 1 pc** W 110 x H 625 x D 500 mm

* When attaching three or more analytical columns or two preparative columns to the column hub, the optional «Column Bracket» is needed.

** If two preparative columns are attached using the column holder SLIM, the optional column clamp ASSY (P/N: 228-17701-94) is required.

For Multiple Detection Triggers
A/D Conversion Board Kit
This is required for preparative work using multiple detector triggers. Expand the hardware to suit the number of detection trigger channels required.

Degassing Units
DGU-403 / DGU-405

A low-capacity degassing unit that uses a special fluororesin membrane.
DGU-403 : 3 flow lines, DGU-405 : 5 flow lines
The maximum operating flow rate per flow line is 10 mL/min.
Designed for use in analytical and preparative fractionation, this unit is used only when retention time reproducibility needs to be improved during analysis.
* When connecting to an LC-20AP, a connection kit must be obtained separately.
* LC-20AR connection kit is required when the operating flow rate is more than 10 mL/min.

Helium Degassing Unit
DGU-10B
Eliminates air bubbles, baseline undulation, drifting, etc. by purging dissolved air from mobile phases.
The DGU-10B can be used to degas up to four mobile phase solutions with helium gas.
This unit is switched ON/OFF from the solvent delivery unit or system controller.

High-Pressure Flow-Line Selection Valves
FCV-20AH2 / FCV-12AH
The valve position is controlled by event signal input.
Valve type: 2-position/6-port rotary valve (recycle valve : 2-position/3-port valve)
Maximum operating pressure: 34.3 MPa
Operating pH range: pH 1 to 10
Operating temperature range: 4 to 35°C
Storing the FCV-12AH in the Option Box helps reduce the volume of preparative piping, including the recycling flow lines.

Low-Pressure Gradient Unit
FCV-200AL
This low-pressure gradient unit is for the LC-20AP large-volume solvent delivery pump.
A gradient can be produced with a single pump, enabling gradient preparative work at low cost.
A single unit is capable of providing up to a four-liquid gradient as well as solvent switching, reducing the work involved in mobile phase investigations during method development.

Reservoir Selection Valves
FCV-11AL / FCV-11ALS / FCV-230AL
Capable of switching solvents using solenoid valves.
The FCV-11AL/FCV-11ALS provide switching between two solvents. The FCV-11AL can supply up to three solvent delivery units, whereas the FCV-11ALS is used for one unit. It can be controlled from the LC-20AP/20AR front panel directly or through a system controller CBM-20A/20Alite and workstation software.
The FCV-230AL provides switching between two solvents (optionally four solvents). It can be controlled from the LC-20AP/20AR front panel directly or through a system controller CBM-20A/20Alite and workstation software.