Principles and Practical Aspects of Preparative Liquid Chromatography

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REFERENCES 1. Huber, U., Solutions for Preparative HPLC, Agilent Application Compendium, publication number 5989-5948EN, 2006 2. Schaffrath, M., von Roedern, E., Hamley, P., Stilz, H.U., High Throughput Purification Of Single Compounds And Libraries, J. Comb. Chem., 2005, 7, 546-553 3. Muhlebach, A., Adam, J., Schon, U., Streamlined approach to high quality purification and identification of compound series using high resolution MS and NMR, J. Sep. Sci., 2011, 34, 2983-2988 4. Koppitz, M., Maximizing Efficiency in the production of compound libraries, J. Comb. Chem., 2008, 10, 573-579 5. Isbell, J., Changing requirements of purification as drug discovery programs evolve from hit discovery, J. Comb. Chem., 2008, 10, 150-157 6. Guth, O., et al., Automated modular preparative HPLC-MS purification laboratory with enhanced efficiency, J. Comb. Chem., 2008, 10, 875-882 7. Penduff, P., Sample Purification Triggered With The Agilent 1260 Infinity Evaporative Light Scattering Detector, Agilent Technologies Technical Overview, publication number 5991-4041EN, 2014 8. The LC Handbook, Agilent Primer, publication number 5990-7595EN, 2013 9. Guillarme, D., et al., Method transfer for fast liquid chromatography in pharmaceutical analysis: Application to short columns packed with small particles. Part II: Gradient experiments, European Journal of Pharmaceutics and Biopharmaceutics, 2008, 68, 430-440 79
10. Schellinger, A.P., Carr, P.W., A practical approach to transferring linear gradient elution methods, Journal of Chromatography A, 2005, 1077, 110-119 11. Schoenmakers, P. J., et al., Gradient Selection in Reversed-Phase Liquid Chromatography. Journal of Chromatography, 1978, 149, 519-537 12. Snyder, L.R., Dolan, J.W., High Performance Gradient Elution, Wiley, 2007 13. Jablonski, J-A.M., Wheat, T.E., Diehl, D.M., Developing focused gradients for isolation and purification, Waters Application Note, reference number Z20002955en, 2009 14. Tei, A., Penduff, P., Guilliet, R., Schulenberg-Schell, H., Using focused gradients on a combined analytical/preparative HPLC system to optimize the scale-up process from 4.6 to 50 mm columns, LCGC Europe, 2013, 26, 315-315 15. Dolan, J.W., Making the Most of a Scouting Run, LCGC North America, 2013, Volume 31, Issue 1, 30-35 16. Penduff, P., Analytical to Preparative HPLC Method Transfer, Agilent Technologies Technical Overview, publication number 5991-2013EN, 2013 80
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PRINCIPLES AND PRACTICAL ASPECTS OF
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CONTENTS Foreword IV Introduction
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FOREWORD As a synthetic chemist, bi
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ABOUT THE AUTHORS Helmut Schulenber
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1 INTRODUCING PREPARATIVE LIQUID CH
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for each compound. Optimized gradie
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Analytical Semi-preparative Prepara
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In contrast, we recommend to use st
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3 COMPONENTS OF A PREPARATIVE LC SY
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Degassing unit Damper Damper Mixer
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Pump Sampling loop Metering device
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3.2.2 Fixed-loop design of autosamp
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Figure 3.11 shows a dual-loop autos
Page 28 and 29:
Moving the switching valve back to
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Plug Plug Sample Figure 3.17 Profil
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When deploying a configuration such
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[Norm.] 7.584 3000 2000 2.791 5.720
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3.3 Flow splitting 3.3.1 T-piece fl
Page 38 and 39: Split ratio = LC flow rate [μL/min
Page 40 and 41: 3.4.1 Matching concentration range
Page 42 and 43: 3.5.1 Collecting fractions manually
Page 44 and 45: 3.5.3.2 Setting slope parameters Th
Page 46 and 47: Flow splitter UV detector ELS detec
Page 48 and 49: UV t D Injection of calibration sam
Page 50 and 51: Figure 3.41 shows the time differen
Page 52 and 53: When acquiring in scan mode a total
Page 54 and 55: 3.7 System considerations 3.7.1 Sys
Page 56 and 57: • Standard 1/16-inch capillaries
Page 58 and 59: [Norm.] 2000 1500 1000 500 v dwell
Page 60 and 61: 4 STRATEGIES FOR SCALE-UP 9-11 4.1
Page 62 and 63: 4.2 Formulas for linear scale-up fr
Page 64 and 65: Figure 4.3 shows the results of a m
Page 66 and 67: 4.3.2 Developing focused gradients
Page 68 and 69: 4.4 Describing the entire scale-up
Page 70 and 71: 4.4.2 Step 2 - Applying a focused g
Page 72 and 73: 5 PRACTICAL GUIDELINES AND DETAILED
Page 74 and 75: 1. Prepare slurry 2. Fill column 3.
Page 76 and 77: 5.2 Determining the system dwell vo
Page 78 and 79: 5.3.1 Simplified procedure for colu
Page 80 and 81: 6. Display UV profile at 242 nm in
Page 82 and 83: [mAU] 1600 1400 1200 1000 4.649 4.0
Page 84 and 85: 5.5.1 Volume overload Figure 5.8 sh
Page 86 and 87: Diameter [cm] 0.46 1.09 2.12 3.00 5
Page 92: www.agilent.com/chem/purification T
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Principles and Practical Aspects of Preparative Liquid Chromatography

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