Separation Techniques in Clinical Chemistry

1 INTRODUCTION......Page 1
CONTENTS......Page 0
2 SAMPLES OF CLINICAL INTEREST......Page 4
2.2 BLOOD: SERUM — PLASMA — WHOLE BLOOD......Page 5
2.6 HUMAN MILK......Page 6
3.1 DISTILLATION......Page 7
3.2 EVAPORATION......Page 10
3.2.1 ROTARY EVAPORATORS......Page 11
4 LIQUID SAMPLE PRETREATMENT......Page 12
4.1 LIQUID–LIQUID EXTRACTION (LLE)......Page 13
4.1.2 COUNTERCURRENT DISTRIBUTION......Page 14
4.1.3 ON-LINE EXTRACTIONS......Page 16
4.1.5 COLUMN EXTRACTION LLE......Page 17
4.2 SOLID-PHASE EXTRACTION (SPE)......Page 18
4.2.1 SPE STEPS......Page 20
4.2.2 SPE SORBENTS......Page 23
4.2.3 SORBENT — ISOLATE INTERACTION......Page 25
4.2.4 SPE PROTOCOL DEVELOPMENT......Page 26
4.2.5 APPLICATIONS IN CLINICAL CHEMISTRY......Page 29
4.2.6 SPE DISC TECHNOLOGY......Page 34
4.2.7 AUTOMATED SOLID- PHASE EXTRACTION SYSTEMS......Page 37
4.3 SOLID-PHASE MICROEXTRACTION (SPME)......Page 41
4.3.1 SPME FIBERS......Page 45
4.3.2 SPME METHOD DEVELOPMENT AND OPTIMIZATION......Page 46
4.3.3 SOLID- PHASE MICROEXTRACTION IN BIOMEDICAL ANALYSIS—DIRECT AND HEADSPACE......Page 47
4.3.4 SPME COUPLED TO HPLC......Page 48
4.3.5 DERIVATIZATION IN SPME......Page 50
4.3.6 ADVANTAGES AND DISADVANTAGES OF SOLID- PHASE MICROEXTRACTION......Page 51
4.4 STIR BAR SORPTIVE EXTRACTION (SBSE)......Page 52
4.5 MEMBRANE-BASED SEPARATIONS......Page 53
4.5.1 MEMBRANES IN SAMPLE FILTRATION......Page 54
4.5.2 DIALYSIS AND MICRODIALYSIS......Page 56
4.5.4 MEMBRANES IN EXTRACTION......Page 58
4.5.5 MICROPOROUS MEMBRANE LIQUID–LIQUID EXTRACTION (MMLLE)......Page 61
4.5.6 MEMBRANE EXTRACTION WITH A SORBENT INTERFACE (MESI)......Page 62
4.5.7 AUTOMATION......Page 63
4.6.2 MOLECULAR IMPRINTED POLYMERS (MIP)......Page 64
4.6.3 RESTRICTED ACCESS MATERIALS (RAM)......Page 66
4.6.4 ON-LINE SAMPLE PREPARATION TECHNIQUE—DIRECT ANALYSIS OF SMALL MOLECULES IN SERUM AND PLASMA......Page 67
5 SOLID SAMPLE PREPARATION......Page 69
5.1 SOLID–LIQUID EXTRACTION......Page 70
5.2 SOXHLET EXTRACTION......Page 71
5.3 FORCED-FLOW LEACHING......Page 72
5.4 SUPERCRITICAL FLUID EXTRACTION (SFE)......Page 73
5.6 MICROWAVE-ASSISTED SOLVENT EXTRACTION (MASE)......Page 76
5.6.1 DYNAMIC MICROWAVE-ASSISTED EXTRACTION (DMAE)......Page 78
5.6.2 FOCUSED MICROWAVE-ASSISTED EXTRACTION......Page 79
5.7 THERMAL DESORPTION......Page 80
5.8 MATRIX SOLID-PHASE DISPERSION (MSPD)......Page 82
6 COLUMN SWITCHING TECHNIQUE......Page 85
7 DERIVATIZATION......Page 88
7.1 DERIVATIZATION IN HPLC......Page 89
7.2 DERIVATIZATION IN GC......Page 91
8 CONCLUSIONS......Page 92
REFERENCES......Page 94
1 INTRODUCTION......Page 103
2 METABOLIC SCREENING AND MASS SPECTROMETRY......Page 104
3 ALTERNATIVE IONIZATION TECHNIQUES FOR MASS SPECTROMETRY......Page 105
4 ELECTROSPRAY TANDEM MASS SPECTROMETRY (ESI-MS/MS)......Page 107
5 APPLICATIONS OF ESI-MS/MS IN BIOCHEMICAL GENETICS......Page 108
5.1 ACYLCARNITINE AND AMINO ACID ANALYSIS......Page 109
5.2 MS/MS-BASED NEWBORN SCREENING......Page 111
5.3 MS/MS-BASED SELECTIVE SCREENING......Page 121
5.4 DETERMINATION OF AMINO ACIDS......Page 122
5.5 ANALYSIS OF ACYLGLYCINES......Page 124
5.6 ANALYSIS OF ORGANIC ACIDS......Page 126
5.7 ANALYSIS OF PURINE AND PYRIMIDINES......Page 129
5.8 ANALYSIS OF BILE ACIDS AND VERY-LONG-CHAIN FATTY ACIDS......Page 130
5.9 ANALYSIS OF STEROIDS......Page 133
5.10 ANALYSIS OF HEXOSE MONOPHOSPHATES AND OLIGOSACCHARIDES......Page 135
5.11 PRENATAL DIAGNOSIS......Page 136
5.12 IN-VITRO LOADING STUDIES......Page 137
5.13 POSTMORTEM DIAGNOSIS......Page 138
REFERENCES......Page 139
1 INTRODUCTION......Page 147
2 SHORT CHARACTERISTIC OF THE METHOD......Page 148
2.1.1 STATIONARY PHASES......Page 149
2.1.2 MOBILE PHASES......Page 151
2.2 SAMPLE PREPARATION AND APPLICATION......Page 152
2.3 DEVELOPMENT TECHNIQUES......Page 153
2.3.2 MULTIPLE DEVELOPMENTS......Page 154
2.3.3 IMMUNOASSAY SEPARATION......Page 155
2.3.4 INSTRUMENTATION OF DEVELOPING PROCESS......Page 156
2.3.5 MULTIMODAL SEPARATION TECHNIQUES......Page 157
2.4 VISUALIZATION AND QUANTITATIVE DETERMINATION......Page 158
2.4.2 PHYSICAL AND PHYSICOCHEMICAL METHODS OF VISUALIZATION; UV MEASUREMENTS......Page 159
2.4.3 BIOLOGICAL–PHYSIOLOGICAL VISUALIZATION......Page 161
2.4.4 MULTIMODAL TECHNIQUES OF DETECTION......Page 163
3.1 AMINO ACIDS......Page 166
3.2.1 SCREENING OF HARD INTOXICATION AND DRUG ABUSE......Page 169
3.2.2 PHARMACOKINETIC STUDIES......Page 172
3.3 CARBOHYDRATES......Page 175
3.4 LIPIDS......Page 176
3.4.1 NEUTRAL LIPIDS......Page 181
3.4.2 COMPLEX LIPIDS......Page 183
3.5 OTHER APPLICATIONS......Page 188
REFERENCES......Page 193
1 INTRODUCTION......Page 202
2 APPLICATION OF CAPILLARY ELECTROPHORESIS IN PHARMACOKINETICS......Page 203
3.1 ANTIVIRAL DRUGS......Page 205
3.5 ANTICOAGULANT DRUGS......Page 206
3.9 PROTEASE INHIBITORS......Page 209
4 APPLICATION OF CE IN THERAPEUTIC DRUG MONITORING......Page 210
4.1 ANTHELMINTHIC DRUGS......Page 211
4.4 ANTIEPILEPTIC DRUGS......Page 212
4.6 AGENTS FOR TREATMENT OF GOUT......Page 215
4.8 CHIRAL DRUGS......Page 216
REFERENCES......Page 223
1 INTRODUCTION......Page 234
2 HISTORICAL......Page 235
3.1 THEORETICAL......Page 236
3.2 PRACTICAL ASPECTS......Page 237
4.2 IMMUNOASSAYS VS. SEPARATION METHODS......Page 239
4.4 PRECISION......Page 240
4.7 ROUTINE VS. RESEARCH IN CHROMATOGRAPHIC ANALYSIS......Page 243
5.1.1 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)......Page 244
5.2 CAPILLARY ELECTROPHORESIS (CE)......Page 245
5.2.2 CONCENTRATION ON THE CAPILLARY......Page 246
6 ADVANCES IN ANALYTICAL TECHNIQUES......Page 247
6.1.2 CHIP TECHNOLOGY......Page 248
7.2 ANALYSIS OF DRUG METABOLITES......Page 249
7.3 CHIRAL SEPARATION......Page 250
7.5 PREDICTING DRUG–MEMBRANE INTERACTIONS......Page 251
7.6 FREE AND BOUND DRUGS......Page 252
8 PHARMACOGENETICS AND TDM......Page 254
9.2 CARDIOACTIVE DRUGS......Page 255
9.4 ANTIBIOTICS......Page 256
9.6 IMMUNOSUPPRESSANTS......Page 259
10 CONCLUDING REMARKS......Page 260
REFERENCES......Page 261
1 STEREOCHEMISTRY......Page 269
2 PHARMACOKINETICS......Page 272
3 PHARMACODYNAMICS......Page 276
4 CHIRALITY AND THERAPEUTIC DRUG MONITORING......Page 279
5.1 B-ADRENOCEPTOR ANTAGONISTS......Page 283
5.4 KETAMINE......Page 284
5.6 NONSTEROIDAL ANTI-INFLAMMATORY DRUGS (NSAIDS)......Page 285
5.9 VERAPAMIL......Page 286
5.11 SINGLE ENANTIOMERS......Page 287
6 THE CONTROVERSY: SINGLE ENANTIOMER VS. RACEMIC THERAPY......Page 288
REFERENCES......Page 290
1 INTRODUCTION......Page 292
1.1 ABSOLUTE BIOAVAILABILITY......Page 294
1.1.1 FIRST-PASS EFFECT......Page 295
2.1 THE ONE-COMPARTMENT MODEL......Page 297
2.2 THE TWO-COMPARTMENT MODEL......Page 299
3 SUBJECTS......Page 300
4.1 HPLC ANALYSIS......Page 301
4.2.2 LIQUID–LIQUID EXTRACTION......Page 302
4.2.3 SOLID-PHASE EXTRACTION......Page 303
4.3.1 SPECTROPHOTOMETRIC DETECTION......Page 304
4.3.3 ELECTROCHEMICAL DETECTION......Page 308
5 PHARMACOKINETIC ANALYSIS......Page 311
6 STATISTICAL ANALYSIS TO ASSESS BIOEQUIVALENCE STUDIES......Page 313
7.1 INTRODUCTION......Page 314
7.2.4 PHARMACOKINETIC AND STATISTICAL ANALYSIS......Page 315
7.3 RESULTS AND DISCUSSION......Page 316
REFERENCES......Page 318
1 INTRODUCTION......Page 321
2 HPLC AND VALIDATION......Page 322
3.2 STEP 2: INSTALLATION QUALIFICATION......Page 324
3.4 STEP 4: PERFORMANCE QUALIFICATION......Page 325
4.3 COLUMN OVEN......Page 326
5 HOLISTIC VALIDATION......Page 327
6.1 SPECIFICITY/ SELECTIVITY......Page 328
6.2 PRECISION (REPEATABILITY)......Page 329
6.3 ACCURACY......Page 332
6.4 LINEARITY......Page 334
6.6 LIMIT OF DETECTION......Page 335
6.9 RUGGEDNESS......Page 336
7.1 GENERAL DESCRIPTION......Page 337
7.2 COLUMN EFFICIENCY......Page 338
7.4 RESOLUTION BETWEEN TWO COMPOUNDS......Page 339
8 WHEN TO VALIDATE?......Page 340
9.1 PRELIMINARY METHOD......Page 341
9.2 CLINICAL METHOD......Page 342
10.1 GENERAL CONDITIONS......Page 343
10.3 PRECISION......Page 344
10.5 LINEARITY AND RANGE......Page 345
11 A FEW WORDS ABOUT GLP......Page 346
REFERENCES......Page 347
1 INTRODUCTION......Page 349
2.1.1 COMPOSITION OF OPIUM AND HEROIN......Page 350
2.1.2 USE OF THE CHROMATOGRAPHIC METHOD FOR ANALYSIS OF ILLICIT HEROIN OF ILLICIT HEROIN......Page 352
2.2.1 FATE OF HEROIN IN THE HUMAN BODY......Page 354
2.2.2 HEROIN METABOLITES AND ASSOCIATED DRUGS IN BODY FLUIDS OF HEROIN ABUSERS......Page 355
2.2.3 OTHER OPIOIDS OF FORENSIC SIGNIFICANCE IN BODY FLUIDS......Page 359
3.1.1 PRODUCTION METHODS OF COCAINE......Page 363
3.2.1 METABOLISM OF COCAINE IN HUMANS......Page 367
3.2.2 ANALYTICAL METHODS FOR COCAINE AND METABOLITES......Page 369
4.1.1 RECENT DEVELOPMENTS ON THE ILLICIT AMPHETAMINE DRUG MARKET......Page 376
4.2.1 METABOLISM AND PHARMACOKINETICS OF PHENETHYLAMINES......Page 377
4.2.2 ANALYSIS OF PHENETHYLAMINES IN BLOOD, PLASMA, AND TISSUES......Page 381
5 CANNABINOIDS......Page 386
5.1 CANNABINOIDS IN PLANT MATERIAL (HASHISH, MARIJUANA)......Page 387
5.2.1 METABOLISM AND PHARMACOKINETICS OF TETRAHYDROCANNABINOL......Page 389
5.2.2 TETRAHYDROCANNABINOL AND METABOLITES IN BLOOD AND URINE......Page 391
5.2.3 TETRAHYDROCANNABINOL AND METABOLITES IN ALTERNATIVE SAMPLES......Page 392
5.2.4 PROBLEMS OF SAMPLE ADULTERATION OR CONTAMINATION......Page 396
REFERENCES......Page 397
1 INTRODUCTION......Page 417
2 LOCALIZATION OF BIOGENIC AMINES......Page 419
3 BIOGENIC AMINES AND NEUROTRANSMISSION......Page 420
4 BIOGENIC AMINES AND BEHAVIORS......Page 422
4.1 DOPAMINE......Page 423
4.2 NOREPINEPHRINE AND EPINEPHRINE......Page 426
4.3 SEROTONIN......Page 428
6 MEASUREMENT OF BIOGENIC AMINES......Page 432
6.2 HISTOCHEMICAL METHODS......Page 433
6.5 ENZYMATIC RADIOCHEMICAL METHODS......Page 434
6.7 POSITRON EMISSION TOMOGRAPHY (PET); EVALUATION OF MONOAMINE SYSTEMS......Page 435
6.9 HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY......Page 436
7 SUMMARY......Page 440
REFERENCES......Page 441
1 INTRODUCTION......Page 449
1.2 PRINCIPLES AND SEPARATION SCHEME......Page 450
2 BORONATE AFFINITY CHROMATOGRAPHY......Page 453
3 LECTIN AFFINITY CHROMATOGRAPHY......Page 455
4 PROTEIN A AND PROTEIN G AFFINITY CHROMATOGRAPHY......Page 457
5 OTHER TYPES OF AFFINITY LIGANDS......Page 458
6.1 OFF-LINE AFFINITY EXTRACTION......Page 459
6.2 ON-LINE AFFINITY EXTRACTION......Page 461
8 AFFINITY-BASED CHIRAL SEPARATIONS......Page 463
8.1 PROTEIN-BASED STATIONARY PHASES......Page 464
8.2 CARBOHYDRATE-BASED STATIONARY PHASES......Page 466
9 CHARACTERIZATION OF BIOLOGICAL INTERACTIONS......Page 467
9.1 ZONAL ELUTION......Page 468
9.2 FRONTAL ANALYSIS......Page 470
10 FUTURE TRENDS AND DEVELOPMENTS......Page 471
REFERENCES......Page 474
1 INTRODUCTION......Page 488
1.1 ANTIBODY STRUCTURE AND PRODUCTION......Page 490
1.2 IAC SUPPORTS AND SOLVENTS......Page 491
2 DIRECT DETECTION OF ANALYTES BY IAC......Page 493
3 CHROMATOGRAPHIC IMMUNOASSAYS......Page 495
3.1 COMPETITIVE BINDING IMMUNOASSAYS......Page 496
3.2 IMMUNOMETRIC ASSAYS......Page 498
4.1 OFF-LINE IMMUNOAFFINITY EXTRACTION......Page 501
4.2 ON-LINE IMMUNOAFFINITY EXTRACTION......Page 503
5 POSTCOLUMN IMMUNODETECTION......Page 505
6 FUTURE TRENDS AND DEVELOPMENTS......Page 506
REFERENCES......Page 508
SEPARATION TECHNIQUES IN CLINICAL CHEMISTRY......Page 515
PREFACE......Page 517
CONTENTS......Page 519
CONTRIBUTORS......Page 521