Elsevier S & T

Lipidomics and Bioactive Lipids: Specialized Analytical Methods and Lipids in Disease: Specialized Analytical Methods and Lipids in Disease

Brown, H. Alex

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Table of contents
  • Contentsv
  • Contributorsxi
  • Prefacexv
  • Volume in Seriesxvii
  • Chapter 1: Liquid Chromatography Mass Spectrometry for Quantifying Plasma Lysophospholipids: Potenti1
  • 1. Introduction2
  • 2. Procedure6
  • 2.1. Materials for liquid chromatography/mass spectrometry/ mass spectrometry6
  • 2.2. Collection of patient samples6
  • 2.3. Extraction of lipids6
  • 2.4. Analysis of incubated plasma7
  • 3. Liquid Chromatography/Mass Spectrometry/Mass Spectrometry7
  • 3.1. Analysis of lysophospholipid recovery rate8
  • 3.2. Standard curve calculation for analysis of plasma8
  • 3.3. Determination of correction factor for LPC isomers9
  • 3.4. Statistical analysis9
  • 4. Discussion9
  • 5. Challenges to the Development of a Clinically Applicable Screening Assay19
  • Acknowledgments21
  • References21
  • Chapter 2: Measurement of Eicosanoids in Cancer Tissues27
  • 1. Introduction28
  • 1.1. COX pathway29
  • 1.2. LOX pathway30
  • 1.3. Cytochrome P-450 pathway31
  • 2. Quantitative Measurement of Eicosanoids32
  • 3. Preparation of Samples33
  • 3.1. Urine samples34
  • 3.2. Plasma preparation34
  • 3.3. Collection of intestinal tumor samples34
  • 3.4. Tissue homogenization34
  • 4. Eicosanoids Extraction35
  • 4.1. Organic solvent extraction35
  • 4.2. Extraction using an octadecylsilyl silica column35
  • 5. Chromatographic Separation of Eicosanoids36
  • 5.1. Thin-layer chromatography36
  • 5.2. Silicic acid column chromatography37
  • 5.3. High-pressure liquid chromatography38
  • 6. Quantitative Analysis of Eicosanoids39
  • 6.1. Radioimmunoassay39
  • 6.2. Enzyme immunoassay40
  • 6.3. Gas chromatography-mass spectrometry41
  • Acknowledgments45
  • References45
  • Chapter 3: Noninvasive Assessment of the Role of Cyclooxygenases in Cardiovascular Health: A Detaile51
  • 1. Introduction52
  • 2. Background and History53
  • 3. Principles of Eicosanoid Analysis by Mass Spectrometry54
  • 3.1. Internal standard54
  • 3.2. Derivatization58
  • 3.3. Extraction58
  • 3.4. Chromatography59
  • 3.5. Mass spectrometry61
  • 3.6. Instrument operational parameters62
  • 4. Urinary Markers of Systemic Eicosanoid Synthesis63
  • 4.1. PGE263
  • 4.2. PGD2 (human)65
  • 4.3. PGD2 (mouse)66
  • 4.4. TxA2 (mouse)66
  • 4.5. TxA2 (human)67
  • 4.6. PGI267
  • 4.7. Isoprostanes69
  • 5. Data Analysis and Interpretation69
  • 6. Concluding Remarks69
  • References71
  • Chapter 4: Lipidomics in Diabetes and the Metabolic Syndrome73
  • 1. Introduction74
  • 2. Brief Introduction of Multi-Dimensional MS-Based Shotgun Lipidomics74
  • 3. Profiling Human Plasma Triacylglycerol Molecular Species77
  • 4. Analysis of Human Heart Lipidome82
  • 5. High Mass Resolution–Based Shotgun Lipidomics for the Analysis of Cardiolipin Molecular Species86
  • Acknowledgment88
  • References89
  • Chapter 5: LC-MS-MS Analysis of Neutral Eicosanoids91
  • 1. Introduction92
  • 1.1. Materials and equipment94
  • 2. Purification of Analytes from Cell Culture Medium and Tissue95
  • 2.1. Endocannabinoids95
  • 2.2. PG-Gs and PG-EAs96
  • 2.3. LC-MS analysis96
  • 3. Quantitation103
  • 3.1. Endocannabinoid recovery105
  • 3.2. PG-EA and PG-G recovery107
  • 4. Linearity and Sensitivity108
  • 5. Postmortem Changes in Analytes109
  • 6. Summary109
  • Acknowledgments110
  • References110
  • Chapter 6: Quantification of F2-Isoprostanes in Biological Fluids and Tissues as a Measure of Oxidan113
  • 1. Introduction114
  • 2. Handling and Storage of Biological Fluids and Tissues for Quantification of F2-IsoPs115
  • 3. Extraction and Hydrolysis of F2-IsoP–Containing Phospholipids in Tissues and Biological Fluids116
  • 4. Purification, Derivatization, and Quantification of Free F2-IsoPs117
  • 5. Application of the Assay to Quantify F2-IsoPs in Biological Tissues and Fluids119
  • 6. Alternative Methods for Measuring F2-IsoPs121
  • 7. F2-Isoprostanes as an Index of Oxidant Stress In Vivo122
  • 8. Summary123
  • Acknowledgments124
  • References124
  • Chapter 7: Measurement of Products of Docosahexaenoic Acid Peroxidation, Neuroprostanes, and Neurofu127
  • 1. Introduction128
  • 2. Handling and Storage of Biological Fluids and Tissues for Quantification of F4-Neuroprostanes132
  • 3. Extraction and Hydrolysis of F4-Neuroprostane-Containing Phospholipids in Tissues and Biological132
  • 4. Purification, Derivatization, and Quantification of F4-Neuroprostanes135
  • 4.1. Analysis of biological samples containing low levels of F4-neuroprostanes137
  • 4.2. Application of the F4-neuroprostane assay in the analysis of CNS tissue and fluids138
  • 4.3. Simultaneous quantification of F2-IsoPs and F4-NPs138
  • 4.4. Quantification of biological samples for neurofurans140
  • 4.5. Optimization of the F4-neuroprostane assay140
  • 5. Summary141
  • Acknowledgments141
  • References141
  • Chapter 8: Enantiomeric Separation of Hydroxy and Hydroperoxy Eicosanoids by Chiral Column Chromatog145
  • 1. Introduction146
  • 2. Chiral Columns, Solvents, and Standards147
  • 2.1. Selection of a chiral column147
  • 2.2. Chiralpak AD and effects of the alcohol modifier148
  • 2.3. Determination of the elution order149
  • 2.4. Preparative synthesis of enantiomeric hydroperoxyeicosatetraenoic acid isomers149
  • 3. Chiral Analyses151
  • 3.1. Hydroperoxy fatty acids using HPLC with UV detection151
  • 3.2. Hydroxy fatty acids using HPLC with UV detection151
  • 3.3. Hydroxy fatty acids using HPLC with mass spectrometric detection153
  • 3.4. Saturated hydroxy–fatty acid derivatives153
  • 3.5. Resolution of prostaglandins and isoprostanes154
  • 3.6. alpha,beta-Unsaturated 4-hydroxy alkenals155
  • 4. Application of Chiral Columns for Separation of Diastereomers155
  • Acknowledgments156
  • References156
  • Chapter 9: Targeted Chiral Lipidomics Analysis by Liquid Chromatography Electron Capture Atmospheric159
  • 1. Introduction160
  • 2. Electron-Capture Atmospheric-Pressure Chemical Ionization161
  • 3. Dissociative Electron Capture162
  • 4. Derivatization for LC-ECAPCI/MS163
  • 5. Procedure164
  • 5.1. Chemicals and materials164
  • 5.2. Extraction of oxidized lipids from cell culture media165
  • 5.3. Extraction of oxidized lipids in the cells or tissues165
  • 5.4. PFB derivatization166
  • 5.5. Mass spectrometry of PFB derivatives166
  • 5.6. Chiral liquid chromatography of PFB derivatives168
  • 5.7. Standard curves and quantitative analysis of oxidized lipids170
  • 6. Summary171
  • Acknowledgments172
  • References172
  • Chapter 10: Shotgun Lipidomics by Tandem Mass Spectrometry under Data-Dependent Acquisition Control175
  • 1. Introduction176
  • 2. Procedure177
  • 2.1. Sample preparation for mass spectrometric analysis177
  • 2.2. Lipid extraction178
  • 2.3. Cholesterol recovery and derivatization178
  • 2.4. Mass spectrometers178
  • 2.5. Data-dependent acquisition setup179
  • 3. Automated Interpretation of MS/MS Spectra Acquired in DDA Experiments181
  • 4. Boolean Scans: A Novel Scan Type Enabled by Postacquisition Data Processing183
  • 5. Comprehensive Characterization of Total Lipid Extracts by DDA-Driven Profiling185
  • 6. Selected Reaction Monitoring in Quantification of Cholesterol and Cholesteryl Esters188
  • Acknowledgments189
  • References190
  • Chapter 11: Identification of Intact Lipid Peroxides by Ag+ Coordination Ion-Spray Mass Spectrometry193
  • 1. Introduction194
  • 2. Analysis of Lipid Oxidation Products196
  • 3. Ag+ Coordination Ion-Spray MS196
  • 4. Identification of Lipid Oxidation Products of Cholestrol Esters by LC-Ag+ CIS-MS198
  • 4.1. Generation of oxidation products from cholesterol arachidonate in vitro198
  • 4.2. Analysis of oxidation products from cholesteryl arachidonate by Ag+ CIS-MS199
  • 4.3. Results200
  • 5. Identification of Intact Lipid Peroxides from Phospholipids by Ag+ CIS-MS204
  • 5.1. Autoxidation of phospholipid 1-palmitoyl-2-linoleoyl-snglycero- 3-phosphocholine (PLPC)205
  • 5.2. LC-CIS-MS analysis of oxidation products from PLPC206
  • 5.3. Results206
  • 6. Precautions of Applying Ag+ CIS-MS to Study Lipids207
  • 7. Conclusions208
  • Acknowledgments209
  • References209
  • Chapter 12: Quantification of Cardiolipin by Liquid Chromatography-Electrospray Ionization Mass Spec213
  • 1. Introduction214
  • 2. Complexity of Cardiolipin Structure217
  • 3. Analysis of Synthetic Cardiolipin Standards Using Liquid Chromatography-Mass Spectrometry218
  • 4. Liquid Chromatography-Mass Spectrometry of Cardiolipins in Total Lipid Extracts221
  • 5. Quantification of Cardiolipin226
  • Acknowledgments228
  • References228
  • Author Index231
  • Subject Index245
Book details
  • Vendor Elsevier S & T
  • SKU 9780123739667
  • ISBN-13 9780080560656
  • Author Brown, H. Alex
  • Category Science
  • Subject Microbiology

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This volume in the well-established Methods in Enzymology series features methods for the study of lipids using mass spectrometry techniques. Articles in this volume cover topics such as Liquid chromatography mass spectrometry for quantifying plasma lysophospholipids: potential biomarkers for cancer diagnosis; Measurement of eicosanoids in cancer tissues; Noninvasive Assessment of the Role of Cyclooxygenases in Cardiovascular Health
A Detailed HPLC/MS/MS Method; Lipidomics in Diabetes and the Metabolic Syndrome; LC-MS-MS Analysis of Neutral Eicosanoids; Quantification Of F2-Isoprostanes In Biological Fluids And Tissues As A Measure Of Oxidant Stress; Measurement of Products of Docosahexaenoic Acid Peroxidation, Neuroprostanes, and Neurofurans; Enantiomeric separation of hydroxy and hydroperoxy eicosanoids by chiral column chromatography; Targeted Chiral Lipidomics Analysis by Liquid Chromatography Electron Capture Atmospheric Pressure Chemical Ionization Mass Spectrometry (LC-ECAPCI/MS); Shotgun Lipidomics by Tandem Mass Spectrometry under Data-Dependent Acquisition Control; Identification of Intact Lipid Peroxides by Ag+ Coordination Ionspray Mass Spectrometry (CIS-MS); Quantification of Cardiolipin by Liquid Chromatography Electrospray Ionization Mass Spectrometry.