Handbooks in Separation Science Series |
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ii | |
Contributors |
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xix | |
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Chapter 1 Sample preparation for liquid chromatography |
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1 | (38) |
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1 | (1) |
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2 | (6) |
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1.2.1 Objectives of Sample Preparation |
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2 | (1) |
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1.2.2 Classification of Sample Preparation |
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3 | (2) |
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1.2.3 Automation of Sample Preparation |
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5 | (3) |
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1.3 Sample Extraction Techniques |
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8 | (21) |
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1.3.1 Liquid-Phase Microextraction |
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8 | (6) |
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1.3.2 Solid-Phase Extraction |
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14 | (4) |
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1.3.3 Solid-Phase Microextraction |
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18 | (2) |
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20 | (4) |
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24 | (3) |
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1.3.6 Other Sorbent Microextraction Techniques for HPLC |
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27 | (2) |
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29 | (10) |
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30 | (9) |
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Chapter 2 Derivatization in liquid chromatography |
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39 | (30) |
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39 | (2) |
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41 | (20) |
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2.2.1 Reagents for UV-Visible Detection |
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43 | (1) |
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2.2.2 Reagents for Fluorescence and Chemiluminescence Detection |
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44 | (6) |
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2.2.3 Reagents for Electrochemical Detection |
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50 | (2) |
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2.2.4 Reagents for Mass-Spectrometric Detection |
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52 | (4) |
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2.2.5 Reagents for the Formation of Diastereomers |
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56 | (3) |
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2.2.6 Multifunctional Reagents for the Formation of Cyclic Derivatives |
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59 | (1) |
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2.2.7 Solid-Phase Analytical Derivatization |
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60 | (1) |
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2.3 Postcolumn Reaction Detectors |
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61 | (2) |
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62 | (1) |
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63 | (6) |
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63 | (6) |
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Chapter 3 Liquid chromatographic separation of enantiomers |
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69 | (18) |
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69 | (2) |
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3.2 Short History of Chiral LC Separations |
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71 | (1) |
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3.3 Materials for LC Separation of Enantiomers |
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72 | (2) |
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3.4 Modes of LC Separation of Enantiomers |
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74 | (4) |
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3.4.1 Analytical Scale Separation of Enantiomers |
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74 | (2) |
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3.4.2 Preparative Scale Separation of Enantiomers in LC |
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76 | (2) |
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3.5 Separation of Enantiomers in Supercritical Fluid Chromatography (SFC) |
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78 | (1) |
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79 | (2) |
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81 | (6) |
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82 | (5) |
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Chapter 4 Amino acid and bioamine separations |
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87 | (20) |
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87 | (1) |
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4.2 Direct Separation of Amino Acids |
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88 | (2) |
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4.2.1 Postcolumn Colorimetric and Fluorescence Derivatization of Amino Acids |
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88 | (1) |
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4.2.2 ESI-MS/MS Determination of Underivatized Amino Acids |
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89 | (1) |
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4.3 Indirect Separation of Amino Acids |
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90 | (5) |
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4.3.1 Derivatization With UV-VIS Reagents |
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90 | (2) |
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4.3.2 Derivatization With Fluorescent Reagents |
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92 | (2) |
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4.3.3 Derivatization for Mass Spectrometric Detection |
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94 | (1) |
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4.4 Enantioselective Liquid Chromatographic Analysis of Amino Acids |
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95 | (3) |
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4.4.1 Chiral Derivatization Reagents for Amino Acid Enantiomers |
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95 | (1) |
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4.4.2 Chiral Stationary Phases for Amino Acid Enantiomers |
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96 | (1) |
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4.4.3 Two-Dimensional Liquid Chromatographic Analysis of Amino Acid Enantiomers |
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96 | (2) |
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4.5 Direct Separation of Biogenic Amines |
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98 | (1) |
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4.6 Indirect Separation of Biogenic Amines |
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99 | (2) |
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101 | (6) |
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101 | (6) |
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Chapter 5 Protein and peptide separations |
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107 | (52) |
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107 | (2) |
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5.2 Methods of Protein Liquid Chromatography |
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109 | (26) |
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5.2.1 Size-Exclusion Chromatography |
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109 | (2) |
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5.2.2 Ion-Exchange Chromatography |
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111 | (5) |
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5.2.3 Methods Based on the Hydrophobic Interaction |
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116 | (7) |
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5.2.4 Affinity Chromatography |
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123 | (6) |
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5.2.5 Chromatography on Hydroxyapatite |
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129 | (1) |
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5.2.6 Chromatography on Monolithic Supports |
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130 | (3) |
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5.2.7 Displacement Chromatography |
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133 | (2) |
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135 | (24) |
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135 | (1) |
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Addendum 1 Protein and Peptide Chromatography---References Update |
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135 | (12) |
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Addendum 2 Sample Displacement Chromatography |
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147 | (1) |
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147 | (2) |
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Development and Use of Sample Displacement Chromatography |
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149 | (1) |
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150 | (2) |
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152 | (5) |
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157 | (2) |
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Chapter 6 Liquid chromatographic separation of oligonucleotides |
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159 | (24) |
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159 | (2) |
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6.2 Oligonucleotide and siRNA Structure and Preparation |
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161 | (4) |
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6.3 Chromatographic Separation of Oligonucleotides |
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165 | (12) |
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6.3.1 Separation of Oligonucleotides With Ion-Exchange Liquid Chromatography |
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166 | (1) |
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6.3.2 Separation of Oligonucleotides With IP-RPLC |
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167 | (7) |
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6.3.3 Separation of Oligonucleotides With Mixed-Mode Chromatography |
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174 | (3) |
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177 | (6) |
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178 | (5) |
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Chapter 7 Separation of glycans and monosaccharides |
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183 | (18) |
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183 | (1) |
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184 | (2) |
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7.3 Analysis and Characterization of Glycans |
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186 | (8) |
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187 | (1) |
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7.3.2 Fluorescent Labeling of Glycans |
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187 | (1) |
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7.3.3 Hydrophilic Interaction Liquid Chromatography |
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188 | (3) |
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7.3.4 Weak Anion-Exchange Liquid Chromatography |
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191 | (1) |
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7.3.5 Exoglycosidase Sequencing |
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192 | (1) |
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7.3.6 Reversed-Phase Liquid Chromatography |
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192 | (1) |
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7.3.7 Porous Graphitic Carbon |
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193 | (1) |
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7.4 Monosaccharide Composition Analysis |
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194 | (5) |
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7.4.1 Hydrolysis of Monosaccharides |
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196 | (1) |
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7.4.2 Labeling and Analysis of Monosaccharides |
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196 | (3) |
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199 | (2) |
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199 | (2) |
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Chapter 8 Separation of lipids |
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201 | (44) |
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8.1 Introduction and Contents |
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202 | (1) |
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8.2 Definitions and Classification |
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203 | (1) |
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8.3 Structures and Occurrence |
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204 | (9) |
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204 | (3) |
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207 | (1) |
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8.3.3 Glycerophospholipids |
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208 | (1) |
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208 | (2) |
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210 | (2) |
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212 | (1) |
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212 | (1) |
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213 | (1) |
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8.4 Sample Handling and Extraction |
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213 | (6) |
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8.4.1 Sampling and Sample Preparation |
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213 | (1) |
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214 | (1) |
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8.4.3 Method of Folch, Lees, and Stanley |
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215 | (1) |
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8.4.4 Method of Bligh and Dyer |
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215 | (1) |
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8.4.5 Accelerated Solvent Extraction |
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216 | (1) |
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8.4.6 Supercritical Fluid Extraction |
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216 | (1) |
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8.4.7 Microwave-Assisted Extraction |
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217 | (1) |
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8.4.8 Other Extraction Methods |
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218 | (1) |
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219 | (20) |
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8.5.1 Thin-Layer Chromatography |
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219 | (3) |
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8.5.2 High-Performance Liquid Chromatography |
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222 | (10) |
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232 | (4) |
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8.5.4 Multidimensional Liquid Chromatography (MDLC, 2DLC) |
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236 | (3) |
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8.6 Conclusions and Future Perspectives |
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239 | (6) |
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239 | (6) |
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Chapter 9 Metabolic phenotyping (metabonomics/metabolomics) by liquid chromatography-mass spectrometry |
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245 | (22) |
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245 | (1) |
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9.2 LC-MS-Based Approaches to Metabolic Phenotyping |
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246 | (10) |
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9.2.1 Reversed-Phase HPLC and U(H)PLC/MS for Metabolic Phenotyping |
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247 | (3) |
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9.2.2 Polar Metabolite Analysis via HILIC, Aqueous Normal Phase (ANP), and Ion Chromatography(IC)/ Ion Exchange (IE) LC-MS-Based Metabolic Phenotyping |
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250 | (2) |
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9.2.3 Multicolumn and Multidimensional LC Separations |
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252 | (2) |
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254 | (2) |
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9.3 Supercritical Fluid Chromatography (SFC) |
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256 | (2) |
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9.4 Ion Mobility Spectrometry |
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258 | (1) |
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259 | (8) |
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260 | (7) |
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Chapter 10 Foodomics: LC and LC-MS-based omics strategies in food science and nutrition |
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267 | (34) |
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267 | (1) |
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10.2 Fundamentals of Omics Approaches Based on LC |
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268 | (9) |
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268 | (3) |
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271 | (2) |
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273 | (2) |
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275 | (1) |
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276 | (1) |
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10.3 LC-Based Foodomics Applications |
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277 | (24) |
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280 | (5) |
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285 | (3) |
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10.3.3 Food Quality, Authenticity, and Traceability |
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288 | (2) |
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290 | (1) |
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290 | (11) |
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Chapter 11 Forensic toxicology |
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301 | (58) |
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11.1 General Drug Screening |
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303 | (4) |
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11.1.1 Extraction Techniques |
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303 | (2) |
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11.1.2 Screening Using Diode Array Detection |
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305 | (2) |
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11.2 Liquid Chromatography-Mass Spectrometry: Background and Considerations |
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307 | (3) |
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11.2.1 Atmospheric Pressure Ionization Sources: APCI, ESI |
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308 | (1) |
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11.2.2 ESI and Mobile Phase pH |
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308 | (1) |
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11.2.3 Atmospheric-Pressure Chemical Ionization |
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309 | (1) |
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11.2.4 General Practical Considerations for LC-MS |
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309 | (1) |
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11.3 Forensic Toxicology LC-MS Applications |
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310 | (8) |
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310 | (2) |
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11.3.2 Single Quadrupole Instruments |
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312 | (1) |
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11.3.3 Time-of-Flight Instruments |
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312 | (1) |
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11.3.4 Orbitrap Analysers |
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313 | (1) |
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11.3.5 Low Resolution Ion Traps |
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314 | (1) |
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11.3.6 Data Dependent Acquisition and Data Independent Acquisition for Broad Screening |
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314 | (4) |
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11.4 LCMS Identification Criteria in Forensic Toxicology |
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318 | (2) |
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11.4.1 The Continuing Relevance of Chromatography |
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318 | (1) |
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11.4.2 MS Identification Criteria |
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319 | (1) |
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11.5 Validation and Matrix Effects |
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320 | (3) |
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11.5.1 Validation Requirements |
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320 | (1) |
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321 | (2) |
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11.6 Testing for Driving Under the Influence of Drugs Using Oral Fluids |
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323 | (6) |
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11.6.1 Analytical Methodology |
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324 | (1) |
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11.6.2 Sample Preparation |
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324 | (1) |
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325 | (3) |
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11.6.4 Liquid Chromatography Analysis of Oral Fluid--Conclusions and Future Directions |
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328 | (1) |
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11.7 Analysis of Novel Psychoactive Substances (NPS) in Forensic Toxicology |
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329 | (3) |
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11.8 Toxicological Analysis of Hair in the Investigation of Drug-Facilitated Crimes |
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332 | (3) |
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11.8.1 Sample Preparation |
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333 | (1) |
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11.8.2 Liquid Chromatography-Tandem Mass Spectrometric Analysis |
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334 | (1) |
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335 | (5) |
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11.9.1 Paraquat and Diquat |
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336 | (1) |
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337 | (1) |
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338 | (1) |
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339 | (1) |
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340 | (19) |
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340 | (18) |
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358 | (1) |
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Chapter 12 Compositional analysis of foods |
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359 | (22) |
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359 | (2) |
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361 | (3) |
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364 | (5) |
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12.3.1 Fat-Soluble Vitamins |
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365 | (1) |
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12.3.2 Water-Soluble Vitamins |
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366 | (2) |
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12.3.3 Multivitamin Methods |
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368 | (1) |
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12.4 Amino Acids, Peptides, and Proteins |
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369 | (1) |
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370 | (2) |
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12.6 Minor Components of Food |
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372 | (2) |
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12.6.1 Phenolic Compounds |
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372 | (1) |
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372 | (1) |
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373 | (1) |
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374 | (3) |
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12.7.1 Food Preservatives |
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374 | (1) |
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375 | (1) |
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375 | (1) |
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376 | (1) |
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12.8 Conclusions and Future Trends |
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377 | (4) |
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377 | (1) |
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378 | (3) |
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Chapter 13 Multiresidue methods for pesticides and related contaminants in food |
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381 | (20) |
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381 | (2) |
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383 | (2) |
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13.3 Matrix Effects in LC-MS Analysis |
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385 | (2) |
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387 | (2) |
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389 | (3) |
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13.6 Individual Methods for Specific Compounds |
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392 | (1) |
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13.7 LC-HR MS in the Field of PRA |
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392 | (9) |
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396 | (5) |
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Chapter 14 Environmental analysis: Persistent organic pollutants |
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401 | (50) |
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14.1 Polycyclic Aromatic Hydrocarbons |
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404 | (5) |
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14.2 Chlorinated Aromatic Compounds |
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409 | (2) |
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411 | (3) |
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14.4 Brominated Flame Retardants |
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414 | (7) |
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415 | (2) |
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14.4.2 HBCDs and Brominated Cycloalkanes |
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417 | (4) |
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14.4.3 Tetrabromobisphenol A |
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421 | (1) |
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14.5 Perfluoroalkyl Compounds |
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421 | (11) |
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14.5.1 Water and Sediments |
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427 | (2) |
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429 | (1) |
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14.5.3 Human Source Materials |
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430 | (2) |
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432 | (4) |
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436 | (1) |
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436 | (15) |
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436 | (13) |
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449 | (2) |
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Chapter 15 Environmental analysis: Emerging pollutants |
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451 | (28) |
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451 | (1) |
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452 | (6) |
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15.2.1 Fast Chromatography |
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453 | (1) |
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15.2.2 On-Line SPE-LC-MS Coupling |
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454 | (1) |
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15.2.3 Multiresidue Methods |
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454 | (2) |
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15.2.4 Suspect Screening and Nontarget Analysis Using LC-HRMS |
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456 | (2) |
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15.3 Target Analysis of Specific Contaminant Groups Using LC-MS |
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458 | (8) |
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15.3.1 Hormones and Other Endocrine Disrupting Compounds (EDCs) |
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458 | (2) |
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15.3.2 Carbon-Based Nanomaterials |
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460 | (1) |
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15.3.3 Perfluoroalkyl and Polyfluoroalkyl Substances |
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461 | (2) |
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463 | (1) |
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463 | (3) |
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466 | (13) |
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467 | (1) |
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467 | (10) |
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477 | (2) |
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Chapter 16 Analysis of natural toxins by liquid chromatography |
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479 | (36) |
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479 | (6) |
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485 | (3) |
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16.3 Lipophilic Marine Toxins |
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488 | (5) |
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493 | (3) |
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496 | (4) |
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16.6 Saxitoxin and Analogs |
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500 | (15) |
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504 | (1) |
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504 | (10) |
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514 | (1) |
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Chapter 17 Liquid chromatography in the pharmaceutical industry |
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515 | (24) |
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17.1 The Role of Separation Science in Pharmaceutical Drug Development |
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515 | (2) |
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17.2 Increasing Chromatographic Resolution |
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517 | (10) |
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17.2.1 High-Resolution Liquid Chromatography Through Increased Efficiency |
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517 | (6) |
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17.2.2 High-Resolution Liquid Chromatography Through Increased Selectivity |
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523 | (4) |
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17.3 Chromatographic Method Development: RPLC |
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527 | (12) |
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17.3.1 Required Method Performance |
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527 | (1) |
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17.3.2 Selection of the Stationary Phase, pH, and Organic Solvent |
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528 | (1) |
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17.3.3 Optimization of Temperature and Gradient |
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529 | (3) |
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17.3.4 Optimization of the Mobile-Phase pH |
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532 | (2) |
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17.3.5 Structure-Driven Prediction of Chromatographic Retention |
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534 | (1) |
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535 | (1) |
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535 | (2) |
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537 | (2) |
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Chapter 18 Determination of veterinary drug residues in foods by liquid chromatography-mass spectrometry: Basic and cutting-edge applications |
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539 | (32) |
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539 | (3) |
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18.1.1 Veterinary Residues |
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539 | (1) |
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18.1.2 Regulatory Aspects in the EU |
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540 | (2) |
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18.2 Options in Veterinary Residue Analysis Using LC-MS |
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542 | (21) |
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18.2.1 Sample Preparation Issues |
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542 | (2) |
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18.2.2 LC Tandem Mass Spectrometry (LC-MS2) |
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544 | (2) |
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18.2.3 LC-High-Resolution Mass Spectrometry (LC-HRMS) |
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546 | (17) |
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563 | (8) |
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564 | (7) |
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Chapter 19 Analysis of vitamins by liquid chromatography |
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571 | (46) |
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571 | (1) |
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19.2 Liquid Chromatographic Determination of Water-Soluble Vitamins |
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572 | (11) |
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574 | (2) |
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576 | (1) |
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577 | (1) |
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578 | (1) |
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578 | (1) |
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579 | (1) |
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580 | (1) |
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581 | (1) |
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582 | (1) |
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19.3 Liquid Chromatographic Determination of Fat-Soluble Vitamins |
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583 | (8) |
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585 | (1) |
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586 | (3) |
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589 | (1) |
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590 | (1) |
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19.4 Multivitamin Methods |
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591 | (26) |
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603 | (14) |
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Chapter 20 Applications of liquid chromatography in the quality control of traditional Chinese medicines: An overview |
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617 | (48) |
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618 | (1) |
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20.2 Separation Modes of Liquid Chromatography |
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619 | (20) |
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20.2.1 Reversed-Phase Liquid Chromatography |
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619 | (12) |
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20.2.2 Hydrophilic Interaction Liquid Chromatography |
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631 | (1) |
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20.2.3 Ion-Exchange Chromatography |
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632 | (1) |
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20.2.4 Size Exclusion Chromatography |
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632 | (4) |
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20.2.5 Two-Dimensional Liquid Chromatography (2DLC) |
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636 | (3) |
|
|
639 | (1) |
|
|
639 | (9) |
|
|
639 | (4) |
|
20.3.2 Nonspectrometry Detection (RID, ELSD, CAD, and ECD) |
|
|
643 | (1) |
|
20.3.3 Multiangle Laser Light Scattering (MALLS) Detection |
|
|
644 | (1) |
|
20.3.4 Mass Spectrometry (MS) Detection |
|
|
644 | (2) |
|
20.3.5 Biochemical Detection (BCD) |
|
|
646 | (1) |
|
|
646 | (2) |
|
|
648 | (17) |
|
|
648 | (17) |
|
Chapter 21 Analysis of neurotransmitters and their metabolites by liquid chromatography |
|
|
665 | (62) |
|
|
|
|
|
|
665 | (12) |
|
21.1.1 Analytical Considerations for Microdialysis |
|
|
668 | (6) |
|
21.1.2 LC Methods for Microdialysis and Tissue Content |
|
|
674 | (3) |
|
|
677 | (12) |
|
|
689 | (2) |
|
|
691 | (5) |
|
21.5 Purines: Adenosine Triphosphate and Adenosine |
|
|
696 | (3) |
|
|
699 | (3) |
|
|
702 | (4) |
|
21.8 Multianalyte Monitoring of Neurotransmitters from Diverse Classes |
|
|
706 | (2) |
|
21.9 Clinical Applications of Microdialysis Sampling and Liquid Chromatographic-Based Analysis |
|
|
708 | (3) |
|
|
708 | (1) |
|
21.9.2 Pharmacokinetic Analysis of Brain Cancer Therapies |
|
|
709 | (2) |
|
|
711 | (16) |
|
|
711 | (16) |
|
Chapter 22 Principles, current applications, and future perspectives of liquid chromatography-mass spectrometry in clinical chemistry |
|
|
727 | (26) |
|
|
|
|
|
727 | (1) |
|
22.2 Sample Preparation in Clinical LC-MS |
|
|
728 | (2) |
|
22.3 LC-MS Technologies in Clinical Chemistry |
|
|
730 | (6) |
|
22.3.1 Liquid Chromatography |
|
|
730 | (3) |
|
|
733 | (1) |
|
22.3.3 Mass Spectrometers |
|
|
734 | (1) |
|
22.3.4 Quadrupole Analyzers |
|
|
735 | (1) |
|
22.3.5 Accurate Mass Analyzers |
|
|
735 | (1) |
|
|
736 | (7) |
|
22.4.1 Fat-Soluble Vitamins |
|
|
736 | (3) |
|
22.4.2 Polyunsaturated Fatty Acids (And Their Metabolites) |
|
|
739 | (2) |
|
22.4.3 Endogenous Glucocorticoids |
|
|
741 | (2) |
|
|
743 | (1) |
|
|
744 | (9) |
|
|
744 | (9) |
|
Chapter 23 Speciation and element-specific detection |
|
|
753 | (16) |
|
|
|
|
753 | (2) |
|
|
755 | (1) |
|
23.3 Sample Storage and Processing |
|
|
755 | (1) |
|
23.4 Speciation Approaches: Direct Methods or Hyphenated Techniques |
|
|
756 | (4) |
|
23.4.1 Separation Techniques |
|
|
756 | (4) |
|
23.5 Interfacing: Nebulizers, Use of Internal Standard and Postcolumn Dilution |
|
|
760 | (1) |
|
23.6 Element-Selective Detection |
|
|
761 | (2) |
|
23.6.1 Atomic Absorption Spectrometry |
|
|
761 | (1) |
|
23.6.2 Inductively Coupled Plasma Detectors |
|
|
761 | (2) |
|
23.7 Quantification and Quality Control |
|
|
763 | (6) |
|
|
765 | (4) |
|
Chapter 24 Environmental analysis: Atmospheric samples |
|
|
769 | (30) |
|
|
|
|
|
769 | (1) |
|
24.2 Sampling and Sample Preparation |
|
|
770 | (3) |
|
|
773 | (17) |
|
|
773 | (5) |
|
|
778 | (1) |
|
24.3.3 Ammonia and Amines |
|
|
779 | (2) |
|
|
781 | (1) |
|
|
782 | (4) |
|
|
786 | (2) |
|
|
788 | (1) |
|
24.3.8 Polycyclic Aromatic Hydrocarbons |
|
|
788 | (1) |
|
|
789 | (1) |
|
24.4 On-Line and On-Site Techniques |
|
|
790 | (2) |
|
|
792 | (7) |
|
|
793 | (1) |
|
|
793 | (6) |
Index |
|
799 | |