
最 低 价:¥991.80
定 价:¥1102.00
作 者:Lloyd R. Snyder, John W. Dolan 著 著
出 版 社:吉林长白山
出版时间:2006-12-1
I S B N:9780471706465
| 作者简介 LLOYD R. SNYDER, PHD, is a Principal at LC Resources in Walnut Creek, California. He is the author or coauthor of several books including An Introduction to Separation Science, Introduction to Modern Liquid Chromatography, Second Edition, and the bestselling Practical HPLC Method Development, Second Edition, all published by Wiley. JOHN W. DOLAN, PHD, is a Principal at LC Resources. He is author of the popular " LC Troubleshooting" column in LCGC Magazine and coauthor with Lloyd Snyder of Troubleshooting LC Systems. |
| PREFACE GLOSSARY OF SYMBOLS AND TERMS 1 INTRODUCTION 1.1 The "General Elution Problem" and the Need for Gradient Elution 1.2 Other Reasons for the Use of Gradient Elution 1.3 Gradient Shape 1.4 Similarity of lsocratic and Gradient Elution 1.4.1 Gradient and Isocratic Elution Compared 1.4.2 The Linear-Solvent-Strength Model 1.5 Computer Simulation 1.6 Sample Classification 1.6.1 Sample Compounds of Related Structure("Regular Samples") 1.6.2 Sample Compounds of Unrelated Structure("Irregular" Samples) 2 GRADIENT ELUTION FUNDAMENTALS 2.1 lsocratic Separation 2.1.1 Retention 2.1.2 Peak Width and Plate Number 2.1.3 Resolution 2.1.4 Role of Separation Conditions 2.1.4.1 Optimizing Retention [Term a of Equation (2.7)] 2.1.4.2 Optimizing Selectivity α [Term b of Equation (2.7)] 2.l.4.3 Optimizing the Column Plate Number N [Term c of Equation (2.7)] 2.2 Gradient Separation 2.2.1 Retention 2.2.1.1 Gradient and Isocratic Separation Compared for "Corresponding" Conditions 2.2.2 Peak Width 2.2.3 Resolution 2.2.3.1 Resolution as a Function of Values of S for Two Adjacent Peaks ("Irregular" Samples) 2.2.3.2 Using Gradient Elution to Predict Isocratic Separation 2.2.4 Sample Complexity and Peak Capacity 2.3 Effect of Gradient Conditions on Separation 2.3.1 Gradient Steepness b: Change in Gradient Time 2.3.2 Gradient Steepness b: Change in Column Length or Diameter 2.3.3 Gradient Steepness b: Change in Flow Rate 2.3.4 Gradient Range ΔФ: Change in Initial Percentage B (Фo) 2.3.5 Gradient RangeΔФ: Change in Final Percentage B (Фf 2.3.6 Effect of a Gradient Delay 2.3.6.1 Equipment Dwell Volume 2.3.7 Effect of Gradient Shape (Nonlinear Gradients) 2.3.8 Overview of the Effect of Gradient Conditions on the Chromatogram 2.4 Related Topics 2.4.1 Nonideal Retention in Gradient Elution 2.4.2 Gradient Elution Misconceptions 3 METHOD DEVELOPMENT 3.1 A Systematic Approach to Method Development 3.1.1 Separation Goals (Step 1 of Fig. 3.1) 3.1.2 Nature of the Sample (Step 2 of Fig. 3.1) 3.1.3 Initial Experimental Conditions 3.1.4 Repeatable Results 3.1.5 Computer Simulation: Yes or No? 3.1.6 Sample Preparation (Pretreatment) 3.2 Initial Experiments 3.2.1 Interpreting the Initial Chromatogram (Step 3 of Fig. 3.1) 3.2.1.1 "Trimming" a Gradient Chromatogram 3.2.1.2 Possible Problems 3.3 Developing a Gradient Separation: Resolution versus Conditions 3.3.1 Optimizing Gradient Retention k* (Step 4 of Fig. 3.1) 3.3.2 Optimizing Gradient Selectivity a* (Step 5 of Fig. 3.1) 3.3.3 Optimizing the Gradient Range (Step 6 of Fig. 3.1) 3.3.3.1 Changes in Selectivity as a Result of Change in k* 3.3.4 Segmented (Nonlinear) Gradients(Step 6 of Fig. 3.1 Continued) 3.3.5 Optimizing the Column Plate Number N*(Step 7 of Fig. 3.1) 3.3.6 Column Equilibration Between Successive Sample Injections 3.3.7 Fast Separations 3.4 Computer Simulation 3.4.1 Quantitative Predictions and Resolution Maps 3.4.2 Gradient Optimization 3.4.3 Changes in Column Conditions 3.4.4 Separation of "Regular" Samples 3.4.5 Other Features 3.4.5.1 Isocratic Prediction (5 in Table 3.5) 3.4.5.2 Designated Peak Selection (6 in Table 3.5) 3.4.5.3 Change in Other Conditions (7 in Table 3.5) 3.4.5.4 Computer-Selection of the Best Multisegment Gradient(8 in Table 3.5) 3.4.5.5 "Two-Run" Procedures for the Improvement of Sample Resolution 3.4.6 Accuracy of Computer Simulation 3.4.7 Peak Tracking …… 4 GRADIENT EQUIPMENT 5 SEPARATION ARTIFACTS AND TROUBLESHOOTING 6 SEPARATION OF LARGE MOLECULES 7 PREPARATIVE SEPARATIONS 8 OTHER APPLICATIONS OF GRADIENT ELUTION 9 THEORY AND DERIVATIONS Appendix Ⅰ THE CONSTANT-S APPROXIMATION IN GRADIENT ELUTION Appendix Ⅱ ESTIMATION OF CONDITIONS FOR ISOCRATIC ELUTION, BASED ON AN INITIAL GRADIENT RUN Appendix Ⅲ CHARACTERIZATION OF REVERSED-PHASE COLUMNS FOR SELECTIVITY AND PEAK TAILING Appendix Ⅳ SOLVENT PROPERTIES RELEVANT TO THE USE OF GRADIENT ELUTION Appendix Ⅴ THEORY OF PREPARATIVE SEPARATION Appendix Ⅵ FURTHER INFORMATION ON VIRUS CHROMATOGRAPHY Index |
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