色譜分析（雙語版）

Chapter 1 The Invention of Chromatography 1
1.1General concepts of analytical chromatography3
1.2The chromatogram5
1.3Gaussian-shaped elution peaks7
1.4The plate theory8
1.5Nernst partition coefficient （K）11
1.6Column efficiency12
1.6.1Theoretical efficiency （number of theoretical plates）12
1.6.2Effective plates number （real efficiency）13
1.6.3Height equivalent to a theoretical plate （HETP）13
1.7Retention parameters14
1.7.1Retention times14
1.7.2Retention volume （or elution volume）14
1.7.3Hold-up volume （or dead volume）14
1.7.4Retention （or capacity）factor15
1.8Separation (or selectivity) factor between two solutes16
1.9Resolution factor between two peaks17
1.10The rate theory of chromatography18
1.10.1Van Deemter’s equation18
1.10.2Golay’s equation20
1.11Optimization of a chromatographic analysis21
1.12Classification of chromatographic techniques23
1.12.1Liquid phase chromatography （LC）23
1.12.2Gas phase chromatography （GC）24
1.12.3Supercritical fluid chromatography （SFC）25
Problems25

第1章 色譜法的發(fā)明 27
1.1分析色譜的一般概念28
1.2色譜圖29
1.3洗脫峰的高斯譜形29
1.4塔板理論29
1.5能斯特分配系數(shù)（K）30
1.6柱效31
1.6.1理論效率（理論塔板數(shù)）31
1.6.2有效塔板數(shù)（真實(shí)效率）32
1.6.3理論塔板高度32
1.7保留參數(shù)32
1.7.1保留時(shí)間32
1.7.2保留體積（或洗脫體積）33
1.7.3死體積33
1.7.4保留因子（或容量因子）33
1.8分離因子（選擇性因子）34
1.9分辨率34
1.10色譜法的速率理論34
1.10.1范第姆特方程35
1.10.2Golay方程36
1.11色譜分析法的優(yōu)化36
1.12色譜技術(shù)的分類37
1.12.1液相色譜（LC）37
1.12.2氣相色譜（GC）37
1.12.3超臨界流體色譜（SFC）38

Chapter 2 Thin Layer Chromatography 39
2.1Principle of TLC39
2.1.1Deposition of the sample39
2.1.2Developing the plate40
2.1.3Identifying the spots41
2.2Characteristics of TLC42
2.3Stationary phases43
2.4Separation and retention parameters44
2.5Quantitative TLC45
Problems47

第2章 薄層色譜法 48
2.1TLC的原理48
2.1.1點(diǎn)樣48
2.1.2薄層板的顯影48
2.1.3斑點(diǎn)的識(shí)別49
2.2TLC的特性49
2.3固定相49
2.4分離和保留參數(shù)50
2.5TLC的定量分析50

Chapter 3 Gas Chromatography 52
3.1Instruments for gas-liquid chromatography53
3.1.1Carrier gas system53
3.1.2Sample injection system55
3.1.3Column configurations and column ovens57
3.1.4Chromatographic detectors57
3.2GC instrument component design59
3.2.1Thermal conductivity detector （TCD）61
3.2.2Flame ionization detector （FID）63
3.2.3Electron capture detector （ECD）64
3.2.4Sulfur-phosphorous flame photometric detector （SP-FPD）67
3.2.5Nitrogen-phosphorous detector （NPD）68
3.3Gas chromatography-mass spectrometry （GC-MS）69
3.3.1Gas chromatography-mass spectrometry73
3.3.2Interface76
3.3.3Recording and analysis77
3.3.4Resolution78
3.4Selection of a stationary phase79
3.4.1Sample classification79
3.4.2Suitable stationary phases80
3.5The scope of GC analysis82
3.6Limitations of GC83
Problems83

第3章 氣相色譜法 85
3.1氣-液色譜儀器85
3.1.1載氣系統(tǒng)85
3.1.2進(jìn)樣系統(tǒng)86
3.1.3色譜柱參數(shù)和柱溫箱86
3.1.4色譜檢測(cè)器87
3.2氣相色譜檢測(cè)器部件的設(shè)計(jì)87
3.2.1熱導(dǎo)檢測(cè)器（TCD）88
3.2.2火焰離子化檢測(cè)器（FID ）89
3.2.3電子捕獲檢測(cè)器（ECD）90
3.2.4硫-磷火焰光度檢測(cè)器（SP-FPD）91
3.2.5氮磷檢測(cè)器（NPD）91
3.3氣相色譜-質(zhì)譜法（GC-MS）92
3.3.1氣相色譜-質(zhì)譜法94
3.3.2接口95
3.3.3記錄和分析95
3.3.4分辨率95
3.4固定相的選擇96
3.4.1樣品分類96
3.4.2選擇合適的固定相97
3.5氣相色譜分析的范圍98
3.6氣相色譜法的局限性98

Chapter 4 High-Performance Liquid Chromatography 99
4.1Instrumentation102
4.1.1Mobile phase reservoir and solvent treatment system102
4.1.2Pumping system104
4.1.3Sample injection system105
4.1.4Columns for HPLC105
4.1.5HPLC detector114
4.1.6LC/MS and LC/MS/MS120
4.2Partition chromatography122
4.2.1Bonded-phase packings122
4.2.2Normal and reversed-phase packings122
4.2.3Choice of mobile and stationary phases124
4.2.4Applications125
4.3Ion chromatography126
4.3.1Ion chromatography based on suppressors127
4.3.2Single-column ion chromatography129
4.4Size-exclusion chromatography129
4.4.1Column packing130
4.4.2Applications130
4.5Affinity chromatography131
4.6Chiral chromatography132
Problems133

第4章 高效液相色譜法 135
4.1儀器135
4.1.1流動(dòng)相儲(chǔ)液瓶和溶劑處理系統(tǒng)136
4.1.2泵系統(tǒng)136
4.1.3進(jìn)樣系統(tǒng)136
4.1.4HPLC柱子137
4.1.5HPLC檢測(cè)器141
4.1.6LC/MS和LC/MS/MS142
4.2分配色譜143
4.2.1鍵合相填料143
4.2.2正相和反相填料143
4.2.3流動(dòng)相和固定相的選擇144
4.2.4應(yīng)用144
4.3離子色譜法145
4.3.1基于抑制柱的離子色譜145
4.3.2單柱離子色譜145
4.4體積排阻色譜146
4.4.1柱填料146
4.4.2應(yīng)用146
4.5親和色譜147
4.6手性色譜147

Chapter 5 Ion Chromatography 148
5.1Basics of ion chromatography148
5.2Stationary phases151
5.2.1Polymer-based materials151
5.2.2Silica-based materials152
5.2.3Resin films153
5.3Mobile phases153
5.4Conductivity detectors155
5.5Ion suppressors156
5.6Quantitative analysis by chromatography158
5.6.1Principle and basic relationship159
5.6.2Areas of the peaks and data treatment software159
5.6.3External standard method160
5.6.4Internal standard method162
5.6.5Internal normalization method164
Problems165

第5章 離子色譜法 169
5.1離子色譜法基礎(chǔ)169
5.2固定相170
5.2.1聚合物基材料170
5.2.2硅膠基質(zhì)材料171
5.2.3樹脂膜171
5.3流動(dòng)相171
5.4電導(dǎo)檢測(cè)器171
5.5離子抑制器172
5.6色譜定量分析173
5.6.1原理與基本關(guān)系173
5.6.2峰面積與數(shù)據(jù)處理軟件173
5.6.3外標(biāo)法174
5.6.4內(nèi)標(biāo)法174
5.6.5內(nèi)標(biāo)歸一化法176

Chapter 6 Size Exclusion Chromatography 177
6.1Principle of SEC177
6.2Stationary and mobile phases179
6.3Calibration curves180
6.4Instrumentation181
6.5Applications of SEC182
6.5.1Molecular weight distribution analysis183
6.5.2Other analysis183
Problems184

第6章 尺寸排阻色譜法 186
6.1SEC的原理186
6.2固定相和流動(dòng)相187
6.3校正曲線187
6.4儀器188
6.5SEC的應(yīng)用188
6.5.1分子量分布分析188
6.5.2其他分析188

Chapter 7 Capillary Electrophoresis and Electrochromatography 189
7.1From zone electrophoresis to capillary electrophoresis189
7.2Electrophoretic mobility and electro-osmotic flow191
7.2.1Electrophoretic mobility-electromigration193
7.2.2Electro-osmotic mobility-electro-osmotic flow193
7.2.3Apparent mobility195
7.3Instrumentation196
7.4Electrophoretic techniques197
7.4.1Capillary zone electrophoresis (CZE)197
7.4.2Micellar electrokinetic capillary chromatography (MEKC)198
7.4.3Capillary gel electrophoresis (CGE)198
7.4.4Capillary isoelectric focusing (CIEF)199
7.5Performance of CE200
7.6Capillary electrochromatography201
Problems207

第7章 毛細(xì)管電泳和電色譜 209
7.1從區(qū)帶電泳到毛細(xì)管電泳209
7.2電泳淌度和電滲流210
7.2.1電泳淌度-電遷移210
7.2.2電滲淌度-電滲流210
7.2.3表觀淌度211
7.3儀器211
7.4電泳技術(shù)212
7.4.1毛細(xì)管區(qū)帶電泳（CZE）212
7.4.2膠束電動(dòng)毛細(xì)管色譜（MEKC）212
7.4.3毛細(xì)管凝膠電泳（CGE）212
7.4.4毛細(xì)管等電聚焦（CIEF）213
7.5CE的效率213
7.6毛細(xì)管電色譜214

Chapter 8 Sample preparation 216
8.1The need for sample pretreatment216
8.2Solid phase extraction (SPE)217
8.3Immunoaffinity extraction219
8.4Microextraction procedures220
8.4.1Solid-phase microextraction (SPME)220
8.4.2Liquid-phase microextraction (LPME)221
8.5Gas extraction on a cartridge or a disc221
8.6Headspace223
8.7Supercritical fluid extraction (SFE)224
8.8Microwave reactors225
Problems226

第8章 樣品制備技術(shù) 227
8.1樣品前處理的必要性227
8.2固相萃取227
8.3免疫親和萃取228
8.4微萃取程序229
8.4.1固相微萃?。⊿PME）229
8.4.2液相微萃取(LPME)229
8.5在卡盒（餅）上進(jìn)行氣體提取229
8.6頂空萃取230
8.7超臨界萃?。⊿FE）230
8.8微波萃取231

Solutions 232

參考文獻(xiàn) 239