| Editor's Preface |
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v | |
| Series Editor's Preface |
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ix | |
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xi | |
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Comparison of various modes and phase systems for analytical HPLC |
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1 | (72) |
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1 | (7) |
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Characteristics of HPLC separation |
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1 | (1) |
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Elution development and chromatographic peaks |
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2 | (1) |
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Basic characteristics of chromatographic separation |
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3 | (2) |
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Retention factor and thermodynamic aspects of chromatography |
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5 | (1) |
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Hydrodynamic (kinetic) aspects of chromatography, band broadening and column efficiency |
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6 | (2) |
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Chromatographic column and column packing particles |
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8 | (5) |
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8 | (2) |
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Packing materials for HPLC |
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10 | (3) |
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13 | (22) |
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Normal-phase chromatography |
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13 | (1) |
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Stationary phases and retention mechanism |
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13 | (1) |
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Retention behaviour in normal-phase chromatography |
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14 | (1) |
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The mobile phase in normal-phase chromatography |
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15 | (3) |
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Reversed-phase chromatography |
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18 | (1) |
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Stationary phases in reversed-phase chromatography |
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19 | (3) |
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Retention behaviour in reversed-phase chromatography |
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22 | (1) |
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The mobile phase in reversed-phase chromatography |
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23 | (1) |
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Retention behaviour of non-ionic solutes in reversed-phase chromatography |
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24 | (2) |
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Reversed-phase chromatography of ionic compounds |
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26 | (3) |
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29 | (2) |
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31 | (1) |
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Ion-exchange chromatography |
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32 | (3) |
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Method development and optimisation of conditions in isocratic HPLC |
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35 | (14) |
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Selection of the separation mode |
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35 | (1) |
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Effects of experimental HPLC conditions on chromatographic resolution |
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36 | (3) |
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Control of the separation efficiency |
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39 | (1) |
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Effect of the temperature on separation |
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40 | (1) |
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Adjustment of the composition of binary mobile phases |
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40 | (1) |
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Selectivity control using ternary or more complex mobile phases |
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41 | (4) |
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Computer-assisted optimisation of HPLC methods |
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45 | (4) |
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Development of gradient-elution separations |
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49 | (20) |
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Gradient-elution versus other HPLC programming techniques |
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49 | (3) |
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Theory of HPLC with binary gradients |
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52 | (1) |
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Gradient elution versus ioscratic elution - effects of the gradient profile on separation |
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53 | (3) |
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Gradient elution in reversed-phase systems |
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56 | (1) |
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Gradient elution in normal-phase and ion-exchange systems |
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57 | (1) |
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Gradient-elution method development |
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58 | (4) |
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Ternary gradients in HPLC |
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62 | (6) |
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Sources of errors in prediction of retention in gradient-elution chromatography |
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68 | (1) |
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69 | (1) |
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69 | (4) |
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Fast Generic HPLC methods |
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73 | (14) |
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73 | (1) |
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74 | (1) |
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Production of fast gradients |
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74 | (1) |
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Strategy for production of fast gradients |
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75 | (7) |
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General strategy for standard bore columns |
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75 | (4) |
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Production of fast gradients with small bore columns |
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79 | (3) |
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Fast gradients in practice |
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82 | (3) |
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85 | (2) |
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Application of standard methods in capillary electrophoresis for drug analysis |
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87 | (20) |
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Introducton to capillary electrophoresis |
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87 | (2) |
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Analysis of pharmaceuticals by CE |
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89 | (1) |
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Low-pH buffer for analysis of basic drugs |
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90 | (2) |
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High-pH buffer for analysis of acidic drugs |
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92 | (1) |
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Micellar electrokinetic chromatography (MEKC) for neutral and/or charged drugs |
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93 | (2) |
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Microemulsion electrokinetic chromatography (MEEKC) for neutral and/or charged drugs |
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95 | (2) |
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Indirect UV detection method for analysis of inorganic anions |
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97 | (3) |
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Indirect UV detection method for analysis of simple organic acids |
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100 | (1) |
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Indirect UV detection method for analysis of metal ions |
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101 | (1) |
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Non-aqueous CE for analysis of acidic and basic drugs |
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102 | (1) |
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Benefits of adopting standard CE methods |
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103 | (2) |
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105 | (2) |
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Chapillary electrochromatography (CEC) |
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107 | (20) |
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107 | (1) |
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Basic principles of capillary electrochromatography |
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108 | (5) |
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108 | (1) |
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Factors that influence electroendosmotic flow (EOF) |
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109 | (1) |
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110 | (2) |
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112 | (1) |
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113 | (1) |
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Stationary phases used in CEC |
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113 | (4) |
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Operational characteristics of CEC |
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117 | (5) |
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117 | (1) |
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118 | (4) |
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Gradient and pressure-assisted (pseudo) CEC |
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122 | (1) |
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123 | (1) |
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123 | (1) |
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124 | (3) |
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Coupled chromatography-mass spectrometry techniques for the analysis of combinatorial libraries |
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127 | (36) |
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127 | (3) |
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Lc/MS analysis of high-throughout parallel synthesis libraries |
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130 | (10) |
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Development of walk-up open-access LC/UV/MS systems |
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132 | (2) |
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134 | (6) |
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Example for monitoring the rehearsal phase of the synthesis of a solid-phase library |
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140 | (4) |
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LC/UV/MS as a pre-screen for autoprep-solution phase |
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144 | (7) |
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Purity profile for phenyl analogue (Fig 5.14) |
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144 | (1) |
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Purity profile for carboxy analogue (Fig 5.15) |
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145 | (6) |
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Purity profile for cyano analogue (Fig. 5.16) |
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151 | (1) |
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Assisted automated LC/MS analysis |
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151 | (1) |
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The analysis of split-pool combinatorial libraries |
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152 | (7) |
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159 | (1) |
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160 | (3) |
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Optimization strategies for HPLC and CZE |
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163 | (50) |
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163 | (2) |
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Responses and response functions |
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165 | (5) |
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Univariate optimization strategies |
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170 | (2) |
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172 | (25) |
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172 | (5) |
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177 | (6) |
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183 | (1) |
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Classical symmetrical designs |
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184 | (4) |
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188 | (4) |
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192 | (5) |
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197 | (4) |
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201 | (2) |
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The simplex sequential approach |
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203 | (6) |
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Automating the whole process: expert systems and knowledge based systems |
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209 | (1) |
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210 | (3) |
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Stragegies for the development of process chromatography as a unit operation for the pharmaceutical industry |
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213 | (80) |
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213 | (4) |
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The process development cycle |
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217 | (8) |
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Process discovery, development and implementation |
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217 | (5) |
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222 | (3) |
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Chromatographic unit operations development |
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225 | (1) |
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Discovery experiment stage |
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225 | (7) |
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228 | (1) |
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228 | (2) |
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Column saturation capacity |
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230 | (1) |
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Relationship between flow rate and plate count |
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231 | (1) |
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232 | (11) |
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Experimental development and modeling |
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233 | (1) |
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234 | (1) |
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235 | (1) |
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236 | (1) |
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237 | (1) |
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Required number of plates |
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237 | (1) |
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Regeneration and equilibration |
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238 | (1) |
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238 | (1) |
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238 | (1) |
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239 | (1) |
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Piping, valves and pressure relief |
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239 | (1) |
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240 | (1) |
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Filtration and guard columns |
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240 | (1) |
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241 | (1) |
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241 | (1) |
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241 | (2) |
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243 | (32) |
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248 | (4) |
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252 | (3) |
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Column saturation capacity |
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255 | (4) |
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259 | (2) |
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261 | (2) |
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263 | (4) |
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267 | (1) |
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267 | (5) |
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272 | (1) |
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273 | (2) |
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275 | (7) |
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Regulatorya and compliance |
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282 | (6) |
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284 | (1) |
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285 | (1) |
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Composition of mobile phase, regeneration solution and local solution |
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285 | (1) |
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286 | (1) |
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Load concentration or volume |
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287 | (1) |
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Cut point location strategy |
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287 | (1) |
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288 | (1) |
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289 | (1) |
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289 | (4) |
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The development and industrial application of automated preparative HPLC |
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293 | (44) |
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293 | (3) |
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Instrumental considerations |
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296 | (3) |
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296 | (1) |
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Stationary phase selection |
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297 | (2) |
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Operating principles and gradient details |
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299 | (1) |
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300 | (11) |
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Analytical scale investigation |
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300 | (1) |
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Preparative scale-up and sample introduction considerations |
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301 | (2) |
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Validation of the preparative chromatography |
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303 | (6) |
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The autoprep purification |
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309 | (2) |
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Practical considerations and `calibrated' methods |
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311 | (16) |
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Problems with the initial generic approach |
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311 | (4) |
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The `calibrated' method for hydrophilic compounds |
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315 | (5) |
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`Calibrated' methods and the advantages of their application |
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320 | (7) |
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Additional system developments |
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327 | (2) |
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329 | (6) |
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The addition of a mass spectrometer |
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329 | (1) |
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Mass spectrometer considerations and chromatography adjustments |
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330 | (2) |
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Instrumental layout and software demands |
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332 | (1) |
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MS-prep system refinements |
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333 | (2) |
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335 | (1) |
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336 | (1) |
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336 | (1) |
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Recent developments in liquid chromatographic enantioseparation |
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337 | (102) |
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337 | (11) |
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Impact of stereochemistry on drug development |
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337 | (1) |
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Historical background of modern liquid-phase enantioseparation |
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338 | (1) |
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Scope and aims of this chapter |
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339 | (1) |
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Mechanism of chiral recognition and enantioseparation |
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339 | (9) |
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Direct enantioseparation by liquid chromatography with chiral stationary phases (CSPs) - chiral selectors and chiral recognition mechanisms |
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348 | (71) |
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Polymeric type selectors and chiral stationary phases |
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350 | (1) |
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Polymeric type CSPs primarily operated in the non-aqueous mobile phase mode |
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350 | (15) |
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Protein type CSPs - representing a class of polymeric type CSPs which can be used with aqueous mobile phases |
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365 | (8) |
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CSPs with macrocyclic, oligomeric and/or intermediate molecular size selectors |
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373 | (1) |
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373 | (8) |
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CSPs with macrocyclic glycopeptide antibiotics as selectors |
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381 | (11) |
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392 | (3) |
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Low molecular weight selectors |
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395 | (1) |
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CSPs based on chiral selectors related to the Pirkle concept |
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395 | (10) |
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405 | (9) |
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Ligand-exchange type CSPs |
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414 | (4) |
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418 | (1) |
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Some aspects of preparative enantioseparation methods |
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419 | (3) |
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Other enantioselecgtive liquid-phase separation techniques |
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422 | (3) |
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425 | (1) |
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Addendum to literature - books on chiral discrimination |
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425 | (1) |
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426 | (13) |
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Basis and pharmaceutical applications of thin-layer chromatography |
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439 | (64) |
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439 | (9) |
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440 | (1) |
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441 | (1) |
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Advantages of planar chromatography |
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442 | (1) |
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443 | (2) |
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Elution, frontal and displacement modes |
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445 | (1) |
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Planar vs. column chromatography |
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446 | (1) |
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Advances in thin-layer chromatography |
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447 | (1) |
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Multidimensional planar chromatography |
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448 | (1) |
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The components of the planar stationary phase |
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448 | (8) |
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Stationary phases for chromatography |
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448 | (1) |
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448 | (2) |
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Inert stationary phase containing silicium dioxides |
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450 | (1) |
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450 | (1) |
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Magnesia (magnesium oxide, magnesium hydroxide) |
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451 | (1) |
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451 | (1) |
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451 | (1) |
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Sephadex and BioGel P gels |
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452 | (1) |
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Chemically modified stationary phases |
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452 | (1) |
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453 | (1) |
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Methods and stationary phases for enantiomeric separations |
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453 | (1) |
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454 | (1) |
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Special additives to the stationary phase |
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454 | (1) |
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454 | (1) |
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455 | (1) |
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455 | (1) |
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Mobile phases for thin-layer chromatography |
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456 | (2) |
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Optimisation of solvent systems |
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457 | (1) |
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458 | (6) |
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458 | (1) |
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Chambers in instrumental TLC |
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459 | (1) |
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Centrifugal thin-layer chromatography |
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459 | (1) |
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High-speed thin-layer chromatography |
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459 | (1) |
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Automated multiple development (AMD) |
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459 | (1) |
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Forced-flow thin-layer chromatography (FF-TLC) |
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460 | (4) |
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464 | (7) |
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464 | (1) |
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Non-destructive detections |
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465 | (2) |
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Detection of TLC with on-line coupled spectroscopic methods other than UV and/or visible monitoring |
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467 | (1) |
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HPTLC-FTIR on-line coupling |
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467 | (1) |
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468 | (1) |
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469 | (1) |
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469 | (1) |
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Electrochemical detection |
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469 | (1) |
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470 | (1) |
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470 | (1) |
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Flame-ionisation detector (FID) |
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471 | (1) |
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Application of TLC in pharmaceutical and forensic analysis |
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471 | (23) |
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Analysis of drugs and metabolities |
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471 | (21) |
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Application of TLC in the study of lipophilicity |
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492 | (2) |
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Quo vadis thin-layer chromatography |
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494 | (4) |
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498 | (1) |
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498 | (5) |
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Recent advances in quantitative structure-retention relationships (QSRR) |
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503 | (32) |
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503 | (2) |
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Strategy of QSRR research |
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505 | (8) |
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506 | (3) |
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509 | (2) |
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Structural descriptors for QSRR |
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511 | (2) |
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513 | (5) |
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Molecular mechanisms of retention in view of QSRR |
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518 | (4) |
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Chromatographic methods of determination of hydrophobicity |
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522 | (2) |
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Applications of QSRR in molecular pharmacology and rational drug design |
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524 | (5) |
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529 | (1) |
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530 | (5) |
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Measurements of physical properties for drug design in industry |
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535 | (50) |
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535 | (1) |
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Measurements of compound lipophilicity using chromatography |
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536 | (13) |
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Measurements of liquid-liquid partition |
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536 | (6) |
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Measurements of chromatographic partition |
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542 | (1) |
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Application of gas chromatography |
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542 | (1) |
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Applicationof thin-layer chromatography (TLC) |
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543 | (1) |
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Application of reversed-phase high-performance liquid chromatography (RP-HPLC) |
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543 | (6) |
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Measuremenrts of members transport by immobilised artificial membrane (IAM) HPLC |
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549 | (3) |
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Measurements of drug-protein binding constants using chromatography |
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552 | (5) |
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Measurements of solubility by HPLC |
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557 | (2) |
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Concentration determination by HPLC for solubility measurements |
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557 | (1) |
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Partition coefficient determination for solubility estimation |
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558 | (1) |
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Measurements of acid-base character (pKa) by HPLC |
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559 | (5) |
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pH dependence of lipophilicity and solubility |
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559 | (2) |
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pH dependence of chromatographic retention |
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561 | (1) |
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Estimation of lipophility of pKa by gradient reversed-phase chromatography |
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562 | (2) |
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Measurements of H-bond acidity, and polarisability-dipolarity by HPLC |
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564 | (16) |
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The importance of H-bond acidity, basicity and polarisability-dipolarity in describing various partition processes and solubility |
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564 | (1) |
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Description of various lipophilicity scales by molecular descriptors (solvation equations) |
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564 | (3) |
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Description of various chromatographic lipophilicity scales by the molecular descriptors |
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567 | (1) |
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Description of solubility by the molecular descriptors |
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568 | (1) |
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Determination of molecular descriptors by chromatography |
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569 | (11) |
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580 | (1) |
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580 | (5) |
| Subject Index |
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585 | |
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