PREPARATIVE CHROM
ATOGRAPHY SOLU
TIONS
PURIFICATIONModular Preparative Chromatography Solutions
from Manual to Fully Automated Systems
PurityNatural Products
Chiral Normal Phase
Peptides
Small molecules
ReversePhase
Oligonucleotides
Scale Up
ImpurityIsolation
Medicinal Chemistry
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NEW
! PLC 2020 Purification System
PLC 2020 Overview Low Pressure High Pressure
Column Type NP Flash Cartridge C18 Flash Cartridge HPLC
Column Size 150 – 340 g 40 – 120 g 10 mm ID 20 mm ID 30 mm ID
Flow Rate 65 – 100 mL/min 40 – 80 mL/min 2 – 10 mL/min 2 – 25 mL/min 2 – 50 mL/min
Loading Capacity 0.3 – 20 g 0.05 – 6 g Up to 0.5 g Up to 2 g Up to 6 g
Injection Volume > 10 mL and solid injection
2 – 10 mL 0.020 – 0.100 mL 0.1 – 10 mL 0.5 – >10 mL
Pressure < 100 psi 1500 – 3500 psi
Calculations based on Methanol/Water solvents - 5 µm column 150 to 250 mm length
Running the System is Simple …
1 Tap Run on the main menu
2 Select Method and then tap Run
3 Load and inject the sample
Wide Range of Purification Modes
Micro-gram to multi-gram sample load capabilities
A fully-functional liquid chromatography purification system, the PLC 2020 Personal Purification System features:
Compact FootprintSimplified HPLC Software
The PLC 2020 Personal Purification System is ideally suited for tailored throughput, high pressure purification needs and is intended to assist an individual or a small group of chemists.
PLC 2020 Purification System LC Out of the Box!
Save Time and Improve EfficiencyHigh Pressure Purification provides superior resolution
Intuitive purification focused interface
Real-time, graphical gradient modifications
Real-time sample tracking during run
Conditional logic fraction collection based on two detector channels using any combination of Slope and/or Level
Auto-Print and Auto-Export of reports at the end of a run
Monitor the progress of the system without being next to it as run lights illuminate the racks during a run, turn off when the run is complete and flash if an error has occurred
Easy-to-Operate Software Fraction Capacity(3 Racks)
Test tubes 13 x 100 mm (240)15 x 45 mm (144)
16 x 100 mm (132)16 x 150 mm (132) 18 x 150 mm (132)
Scintillation vials20 mL (42) 40 mL (42)
Custom racks available
Storage for up to four 4L solvent bottles
Integrated touch- screen control
Three rack positions dedicated to fractions
Interchangeable pump head design to accommodate wide flow rate and pressure range
Selection of up to four solvents
Three USB ports for easy download/upload of methods and results. Easily connect your printer, keyboard and mouse
Column holders for virtually any FLASH and reverse phase columns. Accommodates any FLASH-style cartridge, as well as dry load configurations
High Pressure Reverse PhaseNormal Phase Chiral
Low PressureFLASHSolid Load
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A robust Purification system to last through the years 32
HPLC Purification System
GX Direct Injection Module
Innovative injection port design to reduce void volumes and minimize carryover
Use two modules for analytical and preparative injection
When size matters…
GX series collection options
Low Mount Fraction Collection Separate injection and collection pathways
High Mount Fraction Collection Collection into closed vials and microplates
GX Prep Solvent System
Syringeless technology with access to five off-bed solvents
Injection volumes ranging from 100 µL to tens of mL
Multiple dilution and rinsing solvents
GX Series Bed Capacity
Tube Diameter
GX-281 Sample Quantity(6 Racks)
GX-271 Sample Quantity(5 Racks)
GX-241 Sample Quantity(2 Racks)
10 mm 576 540 216
13 mm 576 400 128
15 mm 576 240 96
16 mm 576 220 88
17 mm 420 220 88
18 mm 420 220 88
25 mm 240 70 -
28 mm 162 70 28
GX-271 Semi-preparative HPLC System
Unique Solutions Built On Specific NeedsLabs and users have different needs and constraints. While others try to provide “one size fits all” solutions, Gilson uses modular components to tailor specific solutions that address current and future needs of our users. Some of the solutions that can be offered include:
Automatic Fraction Re-InjectionThe GX series instruments feature dual injection paths, enabling analytical and preparative injections on a single platform without compromising. TRILUTION LC software can automatically inject the collected fractions for purity confirmation or for secondary purification.
GX-281 Preparative HPLC System
Seamless Automation
Column selection for universal systems:
Analytical method development and Scale Up to Preparative.
Multiple purification modes (RP, NP, Chiral, …)
Purification followed by direct analysis of fractions in analytical.
Column backflush (not shown).
GX Z-Injection Module Sample is aspirated directly into the injection loop for fast injection, decreased cycle times, and low carryover
Analytical to Preparative HPLC System Gilson High Performance Liquid Chromatography (HPLC) systems provide complete solutions for all purification needs. Front-end liquid handlers and autosamplers are available in a range of bed capacities and with footprints optimized for various bench space requirements.
GX Series PlatformsThe GX series platforms feature a selection of bed capacity adapted to the user's throughput needs.
Allow injection and fraction collection on the same instrument
The revolutionary GX Solvent System accommodates sample volumes ranging from microliters to hundreds of milliliters
Numerous injection possibilities ranging from analytical to preparative
Remove Solubility Issues"Sandwich" injection to avoid sample precipitation during the injection process:
Large injection volumes supported through solvent system and 1/8" injection loop.
Fully Automated Sample Pre-Treatment and InjectionLiquid handling and injection capabilities on the same instrument allow multiple injections from the same sample, sample dilution, internal standard addition, sample cleanup by SPE, and more.
GX-241 Semi-preparative HPLC System
Column Selection and Column Back Flush (Selection Set-up Shown)
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Performance, capacity and size to fit every laboratory need… … from mg to gram scale purification 54
HPLC Purification System
Time (minutes)
mVo
lts
% M
obile
Pha
se
210180150120
906030
0-30
100
80
60
40
20
00 2 4 6 8
Retention Time Repeatability
Time (minutes)
Prog
ram
med
Com
posit
ion
(% E
)
Dete
cted
Com
posit
ion
(mAU
)120
100
80
60
40
20
0
300
250
200
150
100
50
00 5 10 15 20 25 30
Gradient Linearity and Accuracy
SpecificationsLight Source
670 nm laser diode, < 5 mWEvaporative Zone Temperature
Ambient – 120˚C
Gas Requirement65 ± 5 psi Nitrogen or Argon
Nebulization Temperature0˚ – 70˚C
Specifications15X 171 172
Wavelength 190 – 700 nm 190 – 720 nm 190 – 610 nm
Pixels - 256 512
Analytical Flow Cell Semi-preparative Flow Cell Preparative Flow Cell
Product # 104445 104441 104443
Internal Volume 12 µL 0.7 µL 0.16 µL
Path length 5 mm 0.2 mm 0.05 mm
Column Size 4 mm – 10 mm 20 mm > 40 mm
Flow Rate 1 – 15 mL/min 15 – 50 mL/min 30 – 200 mL/min
Sample Size 1 µg – 1 mg 1 – 300 mg 300 mg – 15 g
HPLC DetectorsFrom Analytical to Preparative Detection Solutions
Other DetectorsPreparative Refractive Index Detector, Fluorometer, Radioactivity, …
prepELS™ II DetectorThe prepELS™ II Detector is ideal for obtaining the purest fractions, from analytical to preparative, with the ability to detect virtually any analytes with or without a chromophore.
Flow Cell Selection Chart for Optimizing Sensitivity on 15X Series Detectors Selecting the correct flow cell will optimize sensitivity and peak shape.
UV/VIS Detection15X Series UV/VIS DetectorsRugged detectors operate in single wavelength, dual wavelength, or scan wavelength mode.
171/172 Diode Array DetectorsAccurate detectors with an optional remote flow cell design. Ideal for compound identification (spectral library) and peak purity calculations.
The Gilson 506C System Interface allows the collection of analog signals (up to 4) to trigger fraction collection and for reporting.
Gilson offers unsurpassed flexibility in HPLC pumping systems with an extensive product range for a variety of pumping applications.
Adjustable Volume Dynamic mixer, or static mixer ((333/334) and high pressure mixing solvents for optimized gradient performance
Series of Ten Injections
Methyl PB
Ethyl PB
Propyl PB
Average Retention
Time3.44 4.85 6.08
Standard Deviation 0.02 0.02 0.02
CV 0.72% 0.34% 0.29%
Solvent selection of up to four solvents per pump for a total of eight solvents in a binary pumping system
Pump Overview 32X H2 Analytical to Semi Preparative
331/332 Analytical to Semi Preparative
333/334 Analytical to Preparative
Flow Rate 0.3 – 30 mL/min 0.5 – 50 mL/min 1 – 200 mL/min.
Flow Rate Accuracy ± 2% ± 2% ± 1%
Pressure 4300 psi / 300 bar 8700 psi / 600 bar 3040 psi / 210 bars
Column Types ID: 4 — 22 mm from 5 µm particles
ID: 4 — 20 mm from 2.5 µm particles
ID: 4.6 — 50 mm from 5 or 10 µm particles
Typical Application Method development and purification up to 2 grams
Method development, purification up to 6 grams and purity check on fast analytical column
Scale up and purification up to 15 grams
Capable of fast separations with high-efficiency columns in normal and reverse-phase modes, Gilson pumps are the premier solvent delivery solutions for the analytical to preparative chromatography.
Gilson dual-piston pumps for semi preparative and preparative chromatography feature high pressure mixing to guarantee gradient precision and reproducibility.
HPLC PumpsAnalytical, Semi-Preparative, and Preparative Pumping Solutions
Mass Spec Single Quad Settings
PB = Paraben
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NEW
! LC/MS Purification System
Gilson TRILUTION® LC Software graphical sample tracking of sample, chromatogram, and fraction spectra
Mass to beTransferred HPLC
Stream
Mass SpecStream
Mass Transferred
HPLC Stream
Mass Spec Stream
1
3
1
3
4 4
2 2
Aliquot Transfer
Mass to beTransferred HPLC
Stream
Mass SpecStream
Mass Transferred
HPLC Stream
Mass Spec Stream
1
3
1
3
4 4
2 2
Aliquot Fill
MS DetectorQuick-connect
Quick-connect feature allows each user to have a probe, preventing contamination between users in open access environments.
Multiple Mode Operation
Ability to monitor in Full Scan, Extracted Ion and SIM (Selected Ion Monitoring) modes simultaneously.
Source Features
The source features XYZ adjustments of probe positioning to optimize spray in relation to the capillary entrance for higher flows and/or sample concentration and a transparent window for viewing the spray.
Automation & Calibration
Auto Tune and integrated calibration vials for positive and negative ion solutions allow the user to quick optimize the MS.
Rugged & Simple
Simple source maintenance allows for cleaning and maintenance without breaking vacuum—limiting instrument down time and increasing productivity in a rugged design.
Selective Collection of Compounds with Weak UV Response
LC/MS Purification SystemIt’s Your Chemistry… Simplified!
Your time is valuable. The quality of your data is crucial. That’s why Gilson has developed an LC/MS Purification System that is not only extremely easy to use and maintain, but has one of the largest mass ranges in the market today. Operation of the MS is completely integrated into the LC control software, facilitated by a few additional tasks and configuration entries when setting up a method.
Your SpecificationsModular design means each component can be configured to your specifications.
Your Own ProbeQuick-connect probe allows for users to have a dedicated probe. Just walk up and snap in to start, without worry of cross contamination in an open access, multi-user environment.
Your Choice Choose to collect fractions on up to eight data signals using conditional logic based on any combination of UV, DAD, ELSD, and MS.
RUN
Select conditional logic collection to trigger off both UV and MS
Enter target masses and adducts
Select scan range
RUN
Range & Speed
Mass Range 50 – 3,000 amu
Scans Speeds up to 10,000 amu/sec
Mass Based Purification
Simple as:
LC/MS Based Purification... The Ultimate in Efficiency
Save time by collecting only compounds or impurities of interest
Fraction spectra are displayed as they are collected for quick compound verification
Graphical sample tracking of sample, chromatogram, and fraction spectra
Active Splitter
Allows for large, settable split ratio to enable the system to operate with a large flow rate range and column conditions
Split Ratio is Independent of Changes in the HPLC Flow
®
Meeting the growing demand for… …simplified LC/MS based purification solutions 98
Configuration
Fraction Collection Simulator
Fraction Collection Settings
Conditional Fraction Collection
Sample Re-Injection Setup
Apex: Collect the entire peak, but advances to the next tube at the Apex.
Application Run Screen
Graphical Tracking of Sample & Fractions
Switch VALVEMATE Task
Detector Autozero Channel Task
Rinse Probe Task
Stop Fraction Collection Task
Start Fraction Collection Task
Injection Task Fraction Collection Settings Task
TRILUTION® LC SoftwareControl Softw
are
Gilson has redefined purification with our HPLC system control software, TRILUTION®LC. This liquid chromatography software, specifically designed for purification, offers control of the important run and collection parameters necessary to get the required results in terms of separation and recovery even when performing challenging applications.
Full Hardware Control ConfigurationAll aspects of the equipment are set in the configuration tab in the method builder
Drag-and-drop tasks to specific time points for fast and easy method creation
Gradient profile
Hardware control tasks
Fraction collection settings
Advanced Fraction Collection Capabilities Collect by time, volume, level, or slope
Individual parameters for front and back slope
Collection region settings: All, front, tail, APEX
Collect co-eluting peak
Collect non peak
Divide peaks by time or volume
Collect in different tubes for each injection or collect in the same set of tubes for repetitive injections
Conditional Fraction Collection Collect based on data from up to eight channels
Conditional logic using AND, OR, AND/OR
Graphical Fraction Collection OptimizationChange fraction collection parameters
Overlay a chromatogram from a previous run
Simulate the fraction collection
Automatic ProcessingAutomatic sample list generation for post -collection fraction processing such as pooling or re-injection
Automatic sample re-injection based on conditions such as peak area value or size
Visual Operation ListAuto sample list generation
Use of variables for easy scale-up from analytical to preparative runs
Real Time Viewing Real time chromatogram and fraction collection
Real time Fraction Spectra for Mass Spec data
Real Time ActionFull access to all instruments during the run to:
Change gradient profile to elute compounds or end injection
Activate fraction collection, manually advance fraction tubes, and divert to waste
Stop pumps
Graphical Sample Tracking
Identify fraction from chromatogram
Open Access ModuleAdministrator control & permission-setting capabilities
Walk-up user access
Graphical TasksDrag-and-drop tasks to specific time points for quick method creation
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Fraction Collectors
Up to ten programmable time windows can be added for collecting only samples of interest, while discarding the column’s void volume, areas of non-interest and equilibration volumes
3-way diverter valve for collection by slope or level using detector signal
Contact closure inputs are available to remotely start, advance or stop fraction collection
SpecificationsDimensions (w x d x h)
FC 203B: 32.4 x 29.2 x 26.7 cm (12.8 x 11.5 x 10.5 in)
FC 204: 47.9 x 46.4 x 33 cm (18.9 x 18.3 x 13 in)
Valve Switching Speed100 msec
Liquid Contact MaterialPTFE and 316 stainless steel
Max Flow RateFC 203B: 20 mL/min.
FC 204: 20 or 200 mL/min.
FC 203B/FC 204 Fraction Collectors
Multi-column adapter for collecting up to 18 separate channels
Stand alone, compact fraction collectors. Collect by time, drop or peak in tubes, vials or microplates.
Gilson Publications and Education
Gilson HPLC Troubleshooting GuideTroubleshooting High Pressure Liquid Chromatography (HPLC) systems can be straightforward, despite the multiple components. With the helpful forms and checklists in our guide, troubleshooting Gilson HPLC is more simple than ever! Included in this guide are real-life examples using HPLC systems, with real problems and solutions, organized into a sprial bound guide. Eliminate problems that may be related to software, hardware, columns, solvents, or any combination of these. Simple tests to prove purification and reduce or eliminate carryover are also included!
Gilson Application Notes HandbooksThe complimentary Gilson Application Notes Handbooks showcase published applications and scientific advances using Gilson automation and pipettes in a number of different markets from chemists and laboratories around the world. We welcome you to submit your application to us for publishing in our handbooks.
Published applications offer everyone a chance to learn about the recent scientific highlights and new technologies.
Gilson SeminarsAttend our complimentary G.E.T. LIVE Web Seminars to learn about more scientific advances with industry leading applications and technologies from TODAY! Gilson is the host for our guest speakers, who lead the industry with their innovative methods and techniques.
For an archive of our G.E.T. LIVE Web Seminar Recordings, please visit:
http://gilsonwebregistration.podbean.com/gilson-web-seminars-registration-page/
Contact [email protected] or visit www.gilson.com to learn more. It’s FREE!
Choosing a Maintenance Contract from your instrument manufacturer is the best way to:
Service Contracts
The 305 and 307 Pumps are programmable through the incorporated keypad.
SpecificationsFlow Rate
305/306: 10 μL/min – 200 mL/min307: 10 μL/min – 10 mL/min
Accuracy< ± 1%
Reproducibility< 1%
Dimensions (w x d x h)33 x 33 x 15 cm (13 x 13 x 6 in)
Stand alone 30X High Pressure Pumps can be used for:
Repetitive injection of the same sample
Isocratic or Gradient pumping system
Up to 200 mL/min. with interchangeable pump head
Can be incorporated as HPLC pumps or make-up pumps in the standard Gilson HPLC systems under TRILUTION LC Control
Easy maintenance
One or more 306 models can be controlled with a 305 unit for binary or tertiary gradient systems
30X Series HPLC Pumps
HPLC Pumps
Maximize Investment
Increase longevity and reliability of equipment.
Benefit from the expertise of the manufacturer.
Stay informed of any updates.
Control Cost
Budget and plan maintenance.
Preferential and attractive prices.
Guarantee Quality
Certified service engineers performing IQ/OQ.
Comply with manufacturer specifications.
Services & Resources
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Resources
Run Method — FLASH Dry Load
To FLASH Waste
Mobile Phase
Detector
To FLASH
Waste
Mobile Phase
Detector
FLASH Dry LoadFLASH
Separation Scale-up EquationsWhen scaling up from analytical scout runs to preparative purification, the main parameters to scale up are:
)²(Pc2 = Pc1 x Fc2 x Lc2
x Pc1x Dc1
Fc1 x Lc1 Pc2x Dc2
Pc1= Pressure on column 1 (psi)Pc2= Pressure on column 2 (psi)
Concentration Overloading on PLC 2020Saturation of solid phase from on column front change peak shape. Late eluting peak is accelerated by earlier co-eluting compound.
Resources
Gradient Duration (GD)
length preparative (diameter preparative)2 flow rate analytical GD preparative = GD analytical x x x length analytical (diameter analytical)2 flow rate preparative
Flow Rate
Flow rate preparative = mass analytical x length analytical (diameter analytical) 2
length preparative x (diameter preparative) 2
Pressure EquationIn preparative chromatography the back pressure generated by the column and the various tubing can become a constraint. At constant mobile phase viscosity, the pressure drop can be estimated:
Optimizing Preparative HPLCThere are numerous parameters and techniques to optimize preparative HPLC. Optimization will improve chromatography and percent recovery of collected fractions.
Tubing & Column Back Pressure
Tubing Back Pressure (psi/bar) - for 1 meter length
(PEEK) Tubing ID (in/mm - Color Coded)
Flow (mL/min.) 0.005/0.13 — Red 0.010/0.25 — Natural 0.020/0.50 — Or 0.030/0.75 — Green 0.040/1.00 — Stainless
1 378/26 24/1.6
20 472/32 30/2.1 6/0.4
45 13/0.8
120 11/0.8
180 17/1.2
Typical Volume (μL) 13 50 200 450 800
Basic Column Back Pressure - Solvent: Methanol/Water - Solid phase: C18 - 5 μm
Pressure Column ID (mm)
Column Length (mm) 4.6 20 30 50 80
150 1900 psi / 130 bar
250 3100 psi / 213 bar
Typical flow (mL/min.) 1 19 43 118 302
Gilson Preparative Solutions: Automatic Re-injections on short column for purity check
Pumping System Type Column Flow Pressure Quantity
331/332Purification 30 x 250 mm - 5 μm 45 mL/min. 230 bar Up to 6 g
Purity check 2.1 x 50 mm - 2.7 μm 0.8 mL/min. 430 bar
Solid Injection on PLC 2020
Automatic Purity Checking on Gilson SystemAdvantage of dual injection paths and high pressure pumps for analytical and preparative works:
Inject several milliliters or do multiple injections on a preparative column. Then automatically switch to a very selective short analytical column and inject few microliters to quickly check purity of collected fractions. Pure fractions can be pooled to reduce evaporation time.
Mass
mass preparative = mass analytical x length analytical (diameter analytical) 2
length preparative x (diameter preparative) 2
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Gilson, Inc. | P.O. Box 620027 | Middleton, WI 53562-0027 | Tel: 800-445-7661 | Fax: 608-831-7661
www.gilson.com | [email protected] | [email protected] | [email protected] | [email protected] | [email protected]
©2012 Gilson, Inc. All rights reserved. | Specifications subject to change without notice | All trademarks are the property of Gilson, Inc. and it subsidiaries. | LT303061-07
