Lipid Analysis and Lipidomics: NewTechniques and Applications

Lipid Analysis and Lipidomics: New Techniques and Applications......Page 2
Contents......Page 4
Preface......Page 6
Part I. Overview......Page 7
Extraction Methods......Page 8
Classical Applications......Page 10
Thin-Layer Chromatography \0吀䰀䌀......Page 11
High Performance Liquid Chromatography \0䠀倀䰀䌀......Page 13
Gas Chromatography \0䜀䌀......Page 18
Supercritical Fluid Chromatography \0匀䘀䌀......Page 21
Fourier Transform Infrared Spectroscopy \0䘀吀䤀刀......Page 22
Nuclear Magnetic Resonance Spectroscopy \0一䴀刀......Page 23
References......Page 24
Part II. Mass Spectral Techniques/Lipidomics......Page 32
Introduction......Page 33
“Hard” GC-MS-EI and LC-MS-EI......Page 34
“Soft? Gentle Ionization Methods, First Used Mainly for Large Biomolecules Such as Proteins and Peptides, and Well-Suited for Intact Lipids......Page 37
Soft Ionization via FAB-MS......Page 40
Soft Ionization via ESI......Page 41
Soft Ionization via APCI......Page 42
Soft Ionization via APPI......Page 44
Soft Ionization via Matrix Assisted Laser Desorption Ionization-Time of Flight MALDI-TOF......Page 46
Modern Instrumental Approaches for Mass Separation and Detection......Page 48
References......Page 50
Introduction......Page 54
Intrasource Separation of Lipid Classes in Shotgun Lipidomics......Page 56
Identification of Individual Molecular Species of Lipids by 2D MS......Page 62
Quantitation of Lipid Molecular Species by 2D MS......Page 66
Applications of Shotgun Lipidomics in Biological Studies......Page 68
Summary......Page 70
References......Page 71
Introduction......Page 75
Materials and Methods......Page 76
Derativization of Enantiomeric Diacylglycerols DAGs and Monoacylglycerols MAGs......Page 77
Chiral-Phase HPLC of Enantiomeric Hydroxy Fatty Acids......Page 78
Chiral-Phase HPLC of Enantiomeric Glycerolipids......Page 79
Normal Phase HPLC of Diastereomeric DAG Derivatives......Page 80
LC/ESI-MS and MS/MS of Stereoisomeric Lipids......Page 81
Steric Analysis of Monohydroxy Fatty Acids......Page 83
Steric Analysis of Dihydroxy Fatty Acids......Page 90
Steric Analysis of MAGs......Page 91
Steric Analysis of DAGs......Page 93
Steric Analysis of Glycerophospholipids......Page 97
References......Page 104
Materials and Methods......Page 111
Hydroxy and Hydroperoxy Fatty Acids......Page 116
Prostaglandins and Isoprostanes......Page 121
Steryl Ester Hydroxides, Hydroperoxides, Isoprostanes and Core Aldehydes......Page 126
Diradylglycerol Hydroxides, Hydroperoxides, Isoprostanes and Core Aldehydes......Page 130
TAG Hydroxides, Hydroperoxides, Isoprostanes and Core Aldehydes......Page 133
Glycerophospholipid Hydroperoxides, Isoprostanes and Core Aldehydes......Page 139
Acknowledgments......Page 151
References......Page 152
Introduction......Page 159
Conventional Methods for Characterization of UFA Double Bond Position......Page 160
Acetonitrile CACI for FAME Analysis......Page 164
Conclusions......Page 172
References......Page 173
Part III. Chromatographic Techniques......Page 175
Introduction......Page 176
HPLC......Page 177
Gas Chromatography......Page 178
Specific Studies......Page 179
Temperature Effects: TAG and FAME Separations......Page 180
Discussion......Page 184
References......Page 187
Brief History......Page 192
Separation of trans-18:1 as FAMEs......Page 193
Selection of an Internal Standard for Ag+-HPLC Separations......Page 195
Ag+-HPLC Fractionation of trans-18:1......Page 196
Conclusions......Page 201
References......Page 203
Introduction......Page 205
Characteristics of HPSEC in Organic Media......Page 206
Mobile Phase......Page 210
Used Frying Oils......Page 211
Fish Oils......Page 212
Partial Glycerides......Page 213
Fats and Oils Replacers......Page 214
Minor Lipid Compounds......Page 216
Others......Page 217
Methodologies for Concentrated Fractions from Intact Oil Samples......Page 218
Methodology for Concentrated Fractions from FAME......Page 219
Used Frying Fats and Oils......Page 220
Crude and Refined Oils......Page 223
Oxidized Fats and Oils......Page 224
References......Page 226
Introduction......Page 239
Packed vs. Capillary Columns......Page 241
Modifiers......Page 244
Triacylglycerols \0吀䄀䜀, FFA, and Glyceride Mixtures......Page 245
Conclusions......Page 250
References......Page 255
Introduction......Page 260
Principles......Page 261
Quantitation and Applications......Page 262
References......Page 267
Introduction......Page 270
Gas Chromatography......Page 271
Sample Preparation......Page 272
Chromatography......Page 273
Chromatographic Methods......Page 274
Sample Preparation......Page 276
Future Opportunities for Research......Page 280
References......Page 281
Part IV. Vibrational Spectroscopic Techniques......Page 283
Introduction......Page 284
Fatty Acid Structures in Cellular Lipids......Page 285
Cultivation of Cells......Page 286
GC-FID Methodology......Page 287
Application of GC-FID Methodology to Food-Borne Pathogens......Page 288
ATR-FTIR Methodology......Page 291
ATR-FTIR Protocol......Page 292
Multivariate Statistical Analysis of Observed Infrared Spectra......Page 293
Conclusion......Page 294
References......Page 295
Introduction......Page 299
Official GC Methods Available for TFA, but not for CLA Determination......Page 300
Official FTIR Methods for Total TFA, but not for Total CLA Determination......Page 301
FT-NIR and its Applications......Page 302
Gas Chromatography \0䜀䌀......Page 303
FT-NIR Spectral Measurements......Page 305
Results and Discussion......Page 308
FT-NIR Classification of Fats and Oils......Page 310
Typical Classification Report......Page 314
Reason for Using GC as Primary Method and FT-NIR as Secondary Method......Page 316
Development of the FT-NIR Quantification Model......Page 317
Typical GC Separation of FAME and CLA Isomers......Page 321
Present Assessment of the FT-NIR Method for FA Determination and Future Developments Required......Page 324
Conclusion......Page 325
References......Page 326
Oils and Fats, trans and Conjugated Linoleic Acids CLAs......Page 331
Infrared IR Spectrometry in the Determination of trans Fatty Acids and CLAs......Page 332
Chemometrics and Its Application in the Determination of trans Fatty Acids......Page 333
Univariate and Multivariate Calibrations......Page 334
Multivariate Calibration by PLS1 Regression......Page 335
Spectral Measurements and Data Handling......Page 339
Results and Discussion......Page 340
Conclusion......Page 346
References......Page 348
Introduction......Page 351
History and Development of IR Spectroscopy......Page 353
Applications of IR Spectroscopy to Study Protein-Lipid Interactions......Page 354
Differences Between IR and Raman Spectroscopy......Page 358
History and Development of Raman Spectroscopy......Page 359
Applications of Raman Spectroscopy to Study Protein-Lipid Interactions......Page 361
References......Page 367
Part V. Applications......Page 373
Health Issues......Page 374
Chemistry......Page 376
Food Applications......Page 384
Toxicology......Page 386
References......Page 387
Phospholipid Chemical Structures......Page 393
Phospholipid Physical Structures......Page 395
Phase Transitions......Page 396
Heat Capacity......Page 397
Miscibility/Solubility......Page 398
Permeability......Page 399
Dipole Potential......Page 400
Chemical......Page 401
References......Page 408
Structure of Waxes......Page 415
Materials and Methods......Page 416
Structure of Sterols......Page 418
Materials and Methods......Page 422
References......Page 425