Index

Page numbers with “f” denote figures; “t” tables.

A
Accuracy, 60t–61t, 62, 65, 68
Acetylcholine (ACh), 568–573
N-Acetylneuraminic acid, 196
Acidic glycosphingolipids, 214
Acylated glucosamine, 216
Adenosine, 579–581
Adenosine diphosphate (ADP), 579–580
Adenosine monophosphate (AMP), 579–580
Adenosine triphosphate (ATP), 579–581
Adsorption, 96–97
biospecific, 4
protein, 172f
Affinity chromatography, 1–23
analytical, 11–14
basic components of, 3–5
bioaffinity chromatography, 5–6
biomimetic, 9–10
in clinical laboratory, 615–617
DNA, 6
dye-ligand, 9–10
frontal, 13–14
immobilization procedures, 169t–171t
immobilized metal-, 11, 168–173
immunoaffinity chromatography, 6–9
miscellaneous methods of, 14–17
newer developments of, 14–17
protein separation, 166–173
quantitative, 11–12
Affinity ligands, 2–4, 3t
1-(Alkylthio)-2-alkylisoindole, 36–37, 36f
Amino acids, 306–307, 573–579
Amino acids separation, 131–147
direct, 132–135
fluorescamine, postcolumn fluorescence derivatization with, 133f, 134
ninhydrin, postcolumn colorimetric derivatization with, 132–133, 133f
o-phthalaldehyde, postcolumn fluorescence derivatization with, 133–134, 133f
underivatized amino acids, ESI–MS/MS determination of, 134–135
enantioselective HPLC analysis of, 141–144
cinchona-alkaloid-bonded chiral stationary phase, 143
cyclodextrin-bonded chiral stationary phase, 143
(+)-1-(9-fluorenyl)ethyl chloroformate, 143
1-fluoro-2,4-dinitrophenyl-5-l-alanine amide, 141–142
o-phthalaldehyde plus chiral thiols, 142
two-dimensional HPLC analysis of amino acid enantiomers, 143–144
indirect, 135–141
fluorescent reagents, derivatization with, 137–140
mass spectrometry detection, derivatization for, 140–141
UV–Vis reagents, derivatization with, 135–137
2-Aminobenzamide (2AB), 189–190
2-Aminobenzoic acid (2-AA), 189–190, 197–198
2-Aminopyridine (PA), 189–190
3-Aminopyridyl-N-hydroxysuccinimidyl carbamate (APDS), 140–141
6-Aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC), 138, 140
Analyte recovery, determination by perfusion flow rate, 547–550
Analytical affinity chromatography, 11–14
Analytical method risk assessment, 70
Analytical quality-by-design, 64–71
Analytical-scale LC separation, of enantiomers, 82–83
Analytical target profile (ATP), 64–69
example of, 68–69
verification studies, 70
Anandamide, 582–583
Androgens, 216
Anion-exchange chromatography (AEX), 155, 157
Antioxidants, 312–313
Aptamer, 16–17
O-Arachdonylethanolamide, 582–583
D-Araboascorbic acid, See D-isoascorbic acid
2-Arachidonylglycerol (2-AG), 582–583
Argentation chromatography, See Silver-ion liquid chromatography
l-Ascorbic acid (AA), 488–489
Assay for content, 62
Atmospheric-pressure chemical ionization (APCI), 40–41, 115–116
in forensic toxicology, 256–257, 266, 271
lipid analysis by, 232, 239
pesticide-residue analysis by, 324–325
for vitamins analysis, 492, 494–496
Atmospheric-pressure chemical ionization–mass spectrometry (APCI–MS), for fingerprinting analysis, 525
Atmospheric-pressure photoionization (APPI), 238–239
Atmospheric-pressure spray ionization (APSI)
for acetylcholine analysis, 572–573
for adenosine analysis, 583–584
for adenosine triphosphate analysis, 583–584
Atomic absorption spectrometry (AAS), element-selective detection using, 643
Atomic-emission spectrometry, inductively coupled plasma, 644

B

Barrier methods, 104–105
1,2-Benzo-3,4-dihydrocarbazole-9-ethyl chloroformate, 590–591
Beta-2 microglobulin, 627
Bioaffinity chromatography, 5–6
on-line HPLC mining, of active compounds, 532
Bioamines separation
direct, 132–135
fluorescamine, postcolumn fluorescence derivatization with, 133f, 134
ninhydrin, postcolumn colorimetric derivatization with, 132–133, 133f
o-phthalaldehyde, postcolumn fluorescence derivatization with, 133–134, 133f
underivatized amino acids, ESI–MS/MS determination of, 134–135
enantioselective HPLC analysis of, 141–144
cinchona-alkaloid-bonded chiral stationary phase, 143
cyclodextrin-bonded chiral stationary phase, 143
(+)-1-(9-fluorenyl)ethyl chloroformate, 143
1-fluoro-2,4-dinitrophenyl-5-l-alanine amide, 141–142
o-phthalaldehyde plus chiral thiols, 142
two-dimensional HPLC analysis of amino acid enantiomers, 143–144
indirect, 135–141
fluorescent reagents, derivatization with, 137–140
mass spectrometry detection, derivatization for, 140–141
UV–Vis reagents, derivatization with, 135–137
Biogenic amines, 556–568
Biological fingerprinting analysis (BFA), 531–532
Biomarkers
applications in clinical laboratory, 621–623
defined, 621
as tumor markers
Biomimetic affinity chromatography, 9–10
Biosensors, 542–543
for glutamate/GABA analysis, 575t
Biospecific elution, 4–5
Biota, 368–370
Bligh and Dyer method, 220–221
Boron-doped diamond (BDD) electrodes, 580–581
Bovine serum albumin (BSA), 586–587
Brain cancer therapies, pharmacokinetic analysis of, 594–596
Branched-chain fatty acids, 207
Brominated cycloalkanes, 356–359
Brominated diphenylethers (BDEs), 353–356
Brominated flame retardants (BFRs), 339f, 352–360, 393–395
brominated cycloalkanes, 356–359
brominated diphenylethers, 353–356
hexabromocyclododecanes, 356–359
tetrabromobisphenol A (4,4’-isopropylidenebis(2,6-dibromophenol), 359–360
Brominated natural compounds (BNCs), 354–356

C

Capillary electrophoresis (CE), 542–543, 551
amino acid analysis by, 573–574
compositional analysis by, 296
speciation analysis by, 641
Carbohydrates, compositional analysis of, 298–301
Carboxymethylated-aspartic acid (CM-Asp), 11
Cardiolipin, See Diphosphatidylglycerol
Carotenoids, 216
Cation-exchange chromatography (CEX)
protein separation, 153–155, 157
Cause-and-effect matrix, 70
Ceramic hydroxyapatite (CHT), 173
Ceramides, 214
Cerebral ischemia, 593
Chelating ligand, 11
Chemiluminescence detection, reagents for, 31–35
Chemometric analysis, 525–529
Chinese Pharmacopoeia 2010, fingerprinting analysis in, 529–531, 535–536
Chiral LC separations, history of, 77–78
Chiral-phase chromatography, lipid analysis by, 235
Chiral stationary phase (CSP), 76–80, 79t, 82, 85
cinchona-alkaloid-bonded, 143
cyclodextrin-bonded, 143
Chiral thiols plus o-phthalaldehyde, 142
Chlorinated aromatic compounds, 339f, 346–347
4-Chloro-7-nitro-2,1,3-benzoxadiazole, 138–139
Cholesterol, 214–216, 215f
Chromatographic immunoassays, 7–8, 7f
Chromatographic resolution, in liquid chromatography, 433–444
Cibracron Blue 3GA, 9–10, 10f
Cinchona-alkaloid-bonded chiral stationary phase, 143
Cis-9,cis-12,cis-15-octadecatrienoic acid, 209
Cis-9,cis-12-octadecadienoic acid, 209
Cis-9-octadecenoic acid, 207–209, 209f
Clinical chemistry, 611–632
Clinical liquid chromatography
applications of, 620–628
biomarkers, 621–623
proteins, 625–627
therapeutic drug monitoring, 620–621
tissue proteins, 627–628
toxicology, 623–625
detection technologies in, 617–619
electrochemical detection, 617–619
fluorescence, 617
mass spectrometry, 619
UV–visible spectrophotometry, 617
preanalytical specimen handling in, 613, 614t
separation technologies in, 613–617
affinity chromatography, 615–617
ion-exchange chromatography, 615
normal-phase chromatography, 613–615
reversed-phase chromatography, 613–615
Cobalamin, See Vitamin B12
Cold-vapor atomic absorption spectrometry (CVAAS), 643
Collision-induced dissociation (CID), 236–237
Colorants, 313–314
Column length, 434–438
Compositional analysis, of foods, 295–318, 300f
amino acids, 306–307
carbohydrates, 298–301
food additives, 311–314
antioxidants, 312–313
colorants, 313–314
preservatives, 312
future trends of, 314–315
lipids, 307–309
minor components, 309–311
carotenoids, 310–311
phenolic compounds, 309–310
peptides, 306–307
proteins, 306–307
sweeteners, 314
vitamins, 301–306
fat-soluble, 301–303
multivitamin methods, 305–306
water-soluble, 303–305
Comprehensive screens, 624
Concanavalin A (Con A), 5–6
Conjugated dienoic fatty acids, 209
Coordination ion spray, 496
Copolymer-composition distribution (CCD), 107–108
Critical chromatography (CC), 97
Critical pairs, 234
Cyanide, 279–280
Cyanocobalamin, 487–488
Cyclic derivatives formation, multifunctional reagents for, 46–48
Cyclic fatty acids, 209–210
Cyclodextrin-bonded chiral stationary phase, 143

D

Decision limit, 458
l-Dehydroascorbic acid (DHAA), 488–489
Derivatization, in liquid chromatography, 25–56
postcolumn reaction detectors, 49–52
photoreactors, 51–52
reagent selection, 27–49, 28t–30t
chemiluminescence detection, reagents for, 31–38, 35t–36t
cyclic derivatives formation, multifunctional reagents for, 46–48
diastereomers formation, reagents for, 43–46, 44t
electrochemical detection, reagents for, 38–40, 39t
fluorescence detection, reagents for, 31–38, 35t–36t
mass-spectrometric detection, reagents for, 40–43, 42t
solid-phase analytical derivatization, 48–49
UV–visible detection, reagents for, 27–31, 30t, 32t–33t
Detection capability, 458
Diacylglycerols, 210–211
Dialysate extraction fraction, 547
Diastereomers formation, reagents for, 43–46, 44t
Diethylaminoethyl cellulose (DEAE), 193
4-N,N-Dimethylaminoazobenzene-4’-sulfonyl chloride (DABS-Cl), 136–137
1-Dimethylaminonaphthalene-5-sulfonyl chloride (DNS-Cl), 137–138
Diode-array detection (DAD), 458
Diphosphatidylglycerol, 211
Diquat, 278–279
Direct-injection nebulizer (DIN), 642
D-isoascorbic acid (D-IAA), 488
Displacement chromatography, 177–179
DNA affinity chromatography, 6
Dopamine analysis, contemporary techniques for, 569t–570t
Drug abuse, 395–396
Drug-facilitated crimes (DFCs), 274–277
Drug screening, 251–255, 252t
extraction techniques for, 251–252
DUID (driving under the influence of drugs), 258–261, 268–274
Dye-ligand affinity chromatography, 9–10
polymer-shielded, 9–10

E

Electrochemical detection
applications in clinical laboratory, 617–619
reagents for, 38–40, 39t
systems, 542–543
Electrospray deposition interface, 119f
Electrospray ionization (ESI), 14–15, 40–42, 115–116
for acetylcholine analysis, 571–573
for adenosine analysis, 583–584
for adenosine triphosphate analysis, 583–584
in forensic toxicology, 256–257, 266, 271
lipid analysis by, 239
for neuropeptides, 587–589
pesticide-residue analysis by, 324–325
for vitamins analysis, 484, 486–487, 492, 496, 500
Electrospray ionization–mass spectroscopy (ESI–MS), 116
traditional Chinese medicines, analysis of, 521–522
for veterinary drug residues analysis, 460
Electrospray ionization–tandem mass spectroscopy (ESI–MS/MS)
underivatized amino acids, determination of, 134–135
Element-selective detection, 643–645
using atomic absorption spectrometry, 643
Elution
biospecific, 4–5
buffer, 4–5
nonspecific, 4–5
volume, 95
zonal, 12–13
Enantiomers, liquid chromatographic separation of, 75–92
analytical-scale separation, 82–83
chiral LC separations, history of, 77–78
future trends of, 87–88
materials for, 78–80
preparative-scale separation, 83–86
Enantioselective HPLC analysis, of amino acids, 141–144
cinchona-alkaloid-bonded chiral stationary phase, 143
cyclodextrin-bonded chiral stationary phase, 143
(+)-1-(9-fluorenyl)ethyl chloroformate, 143
1-fluoro-2,4-dinitrophenyl-5-l-alanine amide, 141–142
o-phthalaldehyde plus chiral thiols, 142
two-dimensional HPLC analysis of amino acid enantiomers, 143–144
Endocannabinoids, 582–585
Endocrine-disrupting compounds, 396–397
Enzyme purification, 5
Equivalent carbon number (ECN), 232
Erythorbic acid, See D-isoascorbic acid
D-Erythrosphingosine, 213–214
ESI–Fourier-transform ion cyclotron resonance (FTICR) mass spectrometry, 588–589
Essential fatty acid, 209
Estrogen, 216
European Union (EU)
veterinary drug residues, regulatory aspects of, 457–459, 457t
Evaporative light scattering (ELS), 107, 229–231, 300–301, 308
Exoglycosidase sequencing, 193–195
Extraction
liquid–liquid, 251–252, 271, 297–298, 460, 522–523, 583
microwave-assisted, 223, 322
pressurized-fluid, See Accelerated-solvent extraction
solid–liquid, 297–298
solid–phase, 251–252, 271, 281, 296, 302, 306, 322–323, 460–461
supercritical fluid, 221–222, 297–298
techniques, for drug screening, 251–252

F

Failure mode and effects analysis (FMEA), 70
Fast atom-bombardment mass spectrometry (FAB MS), 14–15
Fast chromatography, 391–392
Fast-scan cyclic voltammetry (FSCV), 542–543, 551–553
for adenosine analysis, 579–581
Fat-soluble vitamins, 301–303
liquid chromatography determination of, 489–497, 493f, 501t–509t
vitamin A, 301, 491–492
vitamin D, 301–302, 492–495
vitamin E, 302, 495–496
vitamin K, 302, 496–497
Fatty acids (FAs), 207–210, 208t
branched-chain, 207
conjugated dienoic, 209
cyclic, 209–210
essential, 209
esters, 210
monoenoic, 207–208
oxygenated, 209–210
polyunsaturated, 209
saturated, 207
thia, 210
trans, 208–209
Figures of merit, 551–552
Fingerprinting analysis, 523–531
biological, 531–532
chemometric analysis, 525–529
in Chinese Pharmacopoeia 2010, 529–531, 535–536
multidimensional LC for TCM analysis, 524–525
Fishbone diagram, 70
Flame atomic absorption spectrometry (F AAS), 643
9-Fluorenylmethyl chloroformate, 138, 143, 577
Fluorescamine, postcolumn fluorescence derivatization with, 133f, 134
Fluorescence, 542–543
applications in clinical laboratory, 617
detection, reagents for, 31–35
Fluorescent reagents, derivatization with, 137–140
6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, 138
1-dimethylaminonaphthalene-5-sulfonyl chloride, 137–138
9-fluorenylmethyl chloroformate, 138
4-fluoro-7-nitro-2,1,3-benzoxadiazole, 138–139
4-(1-pyrene)butyric acid N-hydroxysuccinimide ester, 139–140
o-phthalaldehyde, 137
Fluorimetric detection (FLD), 458
1-Fluoro-2,4-dinitrophenyl-5-L-alanine amide (FDAA), 141–142
7-Fluoro-4-nitrobenzoxadiazole (NBD-F), 138–139, 578
Focused microwave-assisted solvent extraction (FMASE), 223
Folacin, 486
Folate, 486
Folch, Lees, and Stanley method, 220
Food additives, 311–314
antioxidants, 312–313
colorants, 313–314
preservatives, 312
sweeteners, 314
Food preservatives, 312
Forensic toxicology, 249–294
drug screening, 251–255
extraction techniques for, 251–252
hair analysis, 274–277
LC–MS/MS in, 276–277
sample preparation, 274–276
LC–MS in, 255–268
applications of, 258–259
atmospheric-pressure chemical ionization, 256–257
continuing relevance of, 264
electrospray ionization, 256–257
mass spectrometric identification criteria, 265–266
matrix effects, 266–268
practical considerations for, 257–258
validation of, 266–268
oral fluid, use of, 268–274
analytical methodology, 269–270
LC–MS/MS in, 271–274
sample preparation, 270–271
targeted poisons, 277–282
cyanide, 279–280
diquat, 278–279
glyphosate, 280–281
paraquat, 278–279
rodenticides, 281–282
Fourier-transform ion cyclotron resonance (FT ICR) mass spectrometry, 236–237
Frontal affinity chromatography (FAC), 13–14
Frontal analysis, See Frontal affinity chromatography
Functionality-type distribution (FTD), 107–108
Functional magnetic-resonance imaging, 542–543

G

Gangliosides, 214
Gas chromatography (GC)
carbohydrate analysis by, 299
compositional analysis of foods, 296
in forensic toxicology, 254–255
Gas chromatography–mass spectrometry (GC–MS), 14–15
for adenosine analysis, 583–584
for adenosine triphosphate analysis, 583–584
in clinical laboratory, 619
in forensic toxicology, 258–261
Gel-filtration chromatography, 151–152
lipid analysis by, 235
Gel-permeation chromatography (GPC), 151–152
lipid analysis by, 235
pesticide-residue analysis by, 323
Glycans, 188–196
exoglycosidase sequencing, 193–195
fluorescent labelling of, 190
HILIC HPLC of, 190–193
PGC HPLC of, 196
release, 189–190
RP HPLC of, 196
types of, 186–188
Glyceroglycolipids, 210–211
Glycerolipids (GLs), 210–211
Glycerophosphoglycerols, 211
Glycerophosphoglycerophosphates, 211
Glycerophosphoglycerophosphoglycerols, 211
Glycerophospholipids (GPs), 211, 212f
Glycoforms, 186
N-Glycolylneuraminic acid, 196
Glycophospholipids, 188
Glycosphingolipids (GSLs), 188, 214
Glyphosate, 280–281
Gradient-elution liquid chromatography (GELC), 112
of polymers, 101–104
Graphite-furnace atomic absorption spectrometry (GF-AAS), 643

H

Hair analysis, 274–277
LC–MS/MS in, 276–277
sample preparation, 274–276
High-performance affinity chromatography (HPAC), 4
High-performance anion-exchange chromatography (HPAEC)
carbohydrate analysis by, 299
High-performance anion-exchange chromatography with pulsed-amperometric detection (HPAEC PAD), 189
High-performance immunoaffinity chromatography (HPIAC), 7
High-performance liquid affinity chromatography (HPLAC), 4
High-performance liquid chromatography (HPLC), 542–543
for adenosine analysis, 579–581
for amino acid analysis, 573–579
for biogenic amines analysis, 564–566
ultra, 565–567
enantioselective analysis, of amino acids
cinchona-alkaloid-bonded chiral stationary phase, 143
cyclodextrin-bonded chiral stationary phase, 143
(+)-1-(9-fluorenyl)ethyl chloroformate, 143
1-fluoro-2,4-dinitrophenyl-5-l-alanine amide, 141–142
o-phthalaldehyde plus chiral thiols, 142
two-dimensional HPLC analysis of amino acid enantiomers, 143–144
high-resolution screening, 532–535
lipid analysis by, 227–235
multidimensional, 240–243
for neurotransmitter analysis
reversed-phase, 552–553, 554t
nonaqueous reversed-phase, 233–235
normal-phase, 228–231
in pharmaceutical industry, 431–454
separation of enantiomers, 76–77
silver-ion, 231–233
traditional Chinese medicines, analysis of, 519–540
for vitamins analysis, 482–483, 485–489, 491, 500
High-performance liquid chromatography–mass spectrometry (HPLC–MS)
data processing, 239–240
lipid analysis by, recent advances in, 235–240
lipidomics, 239–240
High-performance thin-layer chromatography, 225–226
Hofmeister series, anions-cations ordering in, 159f
Hormones, 396–397
Human source materials, 370–372
Hydride-generating atomic absorption spectrometry (HG AAS), 643
Hydrolysis, 219
Hydrophilic interaction HPLC chromatography (HILIC–HPLC), 190–193
for acetylcholine analysis, 571–573
for biogenic amines analysis, 566–567
carbohydrate analysis by, 299–300
in clinical laboratory, 613–615
hair analysis by, 277
lipid analysis by, 235
for neurotransmitter analysis, 554t, 555
for speciation analysis, 640–641
for veterinary drug residues analysis, 461
Hydrophobic-interaction chromatography (HIC)
protein separation, 158–161
Hydrophylic water soluble marine toxins, 415t
Hydroquinones, 216
Hydroxyapatite, chromatography on, 173–174
4-Hydroxycoumarins, 281–282
8-Hydroxyquinoline, 11
Hyphenated techniques, 107–121
Hyphenation techniques, for speciation analysis, 637–641

I

Ichikawa diagram, 70
Identification (ID) test, 62
Identification points (IPs), 458
Iminodiacetic acid (IDA), 11, 12f, 172
Immobilized liposome chromatography (ILC), for fingerprinting analysis, 525
Immobilized metal-affinity chromatography (IMAC), 11, 168–173
Immobolization
covalent, 4
nonspecific, 4
Immunoaffinity chromatography (IAC), 6–9
Immunoassays
chromatographic, 7–8, 7f
competitive binding, 8
noncompetitive binding, 8–9
Immunoglobulin-binding proteins, 6
Immunohistochemical (IHC) assays, 627
Inductively coupled plasma (ICP) detectors, 643–645
atomic-emission spectrometry, 644
mass spectrometry, 644–645
Inductively coupled plasma atomic-emission spectrometry (ICP AES), 644
Inductively coupled plasma mass spectrometry (ICP MS), 644–645
quadrupole, 644–645
sector-field, 644–645
In-source collisionally induced dissociation (ISCID), 261
Interaction chromatography (IC), 107–108
Intermediate precision, 60t–61t, 62
Intraassay precision, See Repeatability
Ion-exchange chromatography
carbohydrate analysis by, 299
in clinical laboratory, 615
compositional analysis by, 306–307
lipid analysis by, 235
protein separation, 153–157
for speciation analysis, 639–640
N-Isobutyryl-d-cysteine (IBDC), 142
N-Isobutyryl-l-cysteine (IBLC), 142
Isocratic liquid chromatography, of polymers, 94–97
Isoprenoids, 216
Isotope-labeled internal standards (ILIS), 325

K

KEGG lipids, 240
Knitted open-tubular (KOT) reactors, 50–52

L

LC–DAD, applications in forensic toxicology, 253–255, 258–261
LC–ESI–MS, compositional analysis by, 307
LC–MS/MS
for acetylcholine analysis, 571–572
for adenosine analysis, 584–585
for adenosine triphosphate analysis, 584–585
applications in forensic toxicology
hair analysis, 276–277
oral fluids, use of, 271–274
for neuropeptides, 587–590
for veterinary drug residues analysis, 461–467
applications of, 462–463
basic principles of, 461–462
LC–nuclear magnetic resonance (LC–NMR) spectroscopy, of polymers, 113–115
LC–TOF MS, pesticide-residue analysis by, 331–333
Lecithin, See Phosphatidylcholine
Lectins, 5–6
Life-cycle management, 64, 71
Ligand(s)
affinity, 2–4, 3t
chelating, 11
Limit of detection (LOD), 267–268, 458
Limits of quantification (LOQs), 63, 458
Limit test, 62
Linearity, 60t–61t, 63
Linoleic acid, 209
LIPID MAPS, 206, 240
Lipidomics, 239–240
analysis by liquid chromatography, 224–243
high-performance liquid chromatography, 227–235
HPLC–MS, 235–240
multidimensional HPLC, 240–243
thin-layer chromatography, 224–227
classification of, 205–206
defined, 205–206
future perspectives of, 243–244
sample extraction and handling, 218–223
accelerated-solvent extraction, 222–223
Bligh and Dyer method, 220–221
Folch, Lees, and Stanley method, 220
microwave-assisted extraction, 223
sample preparation, 218–219
sampling, 218–219
Soxhlet extraction, 219–220
supercritical fluid extraction, 221–222
structures and occurrence of, 206–217
fatty acids, 207–210
glycerolipids, 210–211
glycerophospholipids, 211
polyketides, 217
prenol lipids, 216
saccharolipids, 216
sphingolipids, 213–214
sterol lipids, 214–216
Lipophilic marine toxins, 414t, 418–424, 421t, 423t
Liquid-adsorption chromatography (LAC), 107–108
of polymers, 98–99
Liquid chromatography (LC)
chromatographic resolution in, 433–444
in clinical laboratory, 613
compositional analysis of foods, 296
derivatization in, 25–56
lipid analysis by, 224–243
methods
neurotransmitter analysis by, 552–556
neurotransmitter levels using, 557t–563t
for speciation analysis, 638–641
vitamins analysis by, 477–518
Liquid chromatography at critical conditions (LCCC), 97, 121
of polymers, 99–107
Liquid chromatography at limiting conditions (LC–LC), 104–105
Liquid chromatography at limiting conditions of desorption (LC–LCD), 104–105
Liquid chromatography at the exclusion–adsorption transition point (EATP-LC), 97
Liquid chromatography–Fourier-transform infrared spectroscopy (LC–FTIR), of polymers, 111–113
Liquid chromatography–high-resolution mass spectrometry (LC–HRMS), for veterinary drug residues analysis, 467–471
applications of, 468–469
basic principles of, 467–468
Liquid chromatography–mass spectrometry (LC–MS), 14–15, 41–42
for adenosine analysis, 583–584
for adenosine triphosphate analysis, 583–584
analysis, matrix effects in, 324–325
compositional analysis by, 219
coupling principles, 118f
in forensic toxicology, 255–268
applications of, 258–259
atmospheric-pressure chemical ionization, 256–257
electrospray ionization, 256–257
mass spectrometric identification criteria, 265–266
matrix effects, 266–268
practical considerations for, 257–258
validation of, 266–268
of polymers, 115–121
target analysis of specific contaminant groups using, 393–403
brominated flame retardants, 393–395
drug abuse, 395–396
endocrine-disrupting compounds, 396–397
hormones, 396–397
nanomaterials, 397
perfluorinated compounds, 397–399
pharmaceuticals, 399
sunscreen agents, 401–403
veterinary drug residue in foods, determination of, 455–476, 459f
LC–MS/MS, 461–467, 463t–466t
sample preparation issues, 460–461
Liquid chromatography–size-exclusion chromatography (LC × SEC), 108–111
Liquid–liquid extraction (LLE), 251–252, 271, 297–298, 460, 522–523, 583
Longdan Xiegan Decoction (LXD), for fingerprinting analysis, 525
Lysophosphatidic acid, 211
Lysophosphatidylcholine, 211
Lysophosphatidylserine, 211

M

Magnetic-resonance imaging (MRI), 542–543
Martin’s rule, 96–97
Mass-spectrometric detection, reagents for, 40–43, 42t
Mass spectrometric identification criteria, in forensic toxicology, 265–266
Mass spectrometry (MS), 542–543
amino compounds detection, derivatization for, 140–141
6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, 140
3-aminopyridyl-N-hydroxysuccinimidyl carbamate, 140–141
in clinical laboratory, 619
fast atom-bombardment, 14–15
gas chromatography–mass spectrometry, 14–15
inductively coupled plasma, 644–645
matrix-assisted laser desorption–ionization time-of-flight, 14–15
surface-noncovalent-affinity, 15
Matrix-assisted laser desorption–ionization–mass spectrometry (MALDI–MS), 115–117
coupling with liquid chromatography, 117–120
Matrix-assisted laser desorption–ionization time-of-flight mass spectrometry (MALDI–TOF MS), 14–15
compositional analysis by, 307
Matrix effects, 266–268
Metal-chelate affinity chromatography (MCAC), See Immobilized metal-affinity chromatography
Metanephrines, applications in clinical laboratory, 622–623
Method-control strategy, establishment of, 70–71
Method development, 69–70
Method-operable design region (MODR), 64
establishment of, 70
Method validation, 57–74
analytical method risk assessment, 70
analytical target profile, 65–69
example, 68–69
verification studies, 70
guidelines for, 59t
life-cycle management, 71
method-control strategy, establishment of, 70–71
method-operable design region, establishment of, 70
for pesticide-residue analysis, 325–327
quality-by-design, 64–71
analytical, 64–71
technique selection for, 69–70
traditional, 58–64
Method verification, 449–451
Methylmalonic acid (MMA), applications in clinical laboratory, 622
Methylmalonic acidemias, 622
Microconcentric nebulizers (MCNs), 642
Microdialysis, 542–544, 543f
analytical considerations for, 547–552
analyte recovery, determination by perfusion flow rate, 547–550
figures of merit, 551–552
microdialysis sampling, temporal resolution of, 550–551
clinical applications of, 592–596
brain cancer therapies, pharmacokinetic analysis of, 594–596
cerebral ischemia, 593
for dopamine analysis, 547
for glutamate/GABA analysis, 575t
liquid chromatography methods for, 552–556
probes
calibration of, 549–550
concentric, 544f
Microwave-assisted extraction (MAE), 223, 322
Minimum required performance limit (MRPL), 458
Minor components, of food, 309–311
carotenoids, 310–311
phenolic compounds, 309–310
Mobile-phase pH, 256–257
optimization, 448–452
Molecularly imprinted polymers (MIPs), 15–16, 16f
Molecular sieve chromatography, 151–152
Monoacylglycerols, 210–211
Monoenoic fatty acids, 207–208
Monolithic supports, chromatography on, 175–177
Monosaccharides
composition analysis, 196–200
hydrolysis of, 197–198
labeling of, 198–200
Multicompound quantitation, 521–523
Multidimensional high-performance liquid chromatography, 240–243
Multidimensional liquid chromatography (MDLC), 164
TCM analysis by, 524–525
Multiple-reaction monitoring (MRM) transition, 572–573
Multiresidue methods, 392–393
Multivariate data analysis (MVDA), 112
Multivitamin methods
for compositional analysis, 305–306
liquid chromatography determination of, 497–500
Mycotoxins, 411–412, 413t

N

Nanomaterials, 397
Naphthalene-2, 3-dicarboxaldehyde (NDA), 574–577
N-Arachinonoyldopamine (NADA), 582–583
Natural toxins, analysis of, 411–430
analogs, 425–426
lipophilic marine toxins, 418–424, 421t, 423t
saxitoxin, 425–426
tetrodotoxin, 415–418, 417t
Nebulizer(s)
direct-injection, 642
microconcentric, 642
ultrasonic, 642
use of internal standard–postcolumn dilution, 641–643
Neuropeptides, 585–590
Neurotransmitters, 541–610
from diverse classes, multianalyte monitoring of, 590–592
LC-based analysis, clinical applications of, 592–596
microdialysis, 542–543
analytical considerations for, 547–552
clinical applications of, 592–596
liquid chromatography methods for, 552–556
Neutral glycosphingolipids, 214
Neutral lipids, 205–206
Niacin, See Vitamin B3
Ninhydrin (2,2-dihydroxyindane-1,3-dione), postcolumn colorimetric derivatization with, 132–133, 133f
Nitrilotriacetic acid (NTA), 11, 12f, 172
4-Nitrobenzo-2-oxa-1,3-diazole (NBD), 138–139
Nonaqueous reversed-phase (NARP) liquid chromatography, 233–235
vitamins analysis by, 491
Normal-phase high-performance liquid chromatography (NP HPLC), 228–231
Normal-phase liquid chromatography (NP LC)
applications in clinical laboratory, 613–615
compositional analysis by, 219
Normetanephrines, applications in clinical laboratory, 622–623
Nuclear magnetic resonance (NMR), 635

O

Octadecaenoic acid, 207
Oleic acid, 207–208, 209f
One-site immunometric assay, 8
On-line HPLC mining, of active compounds, 531–535
bioaffinity chromatography, 532
HPLC high-resolution screening, 532–535
On-line SPE–LC–MS coupling, 392
Opioids assays, 624–625
Oral fluid, use of, in forensic toxicology, 268–274
analytical methodology, 269–270
LC–MS/MS in, 271–274
sample preparation, 270–271
Orbitrap, 236–237, 262, 265
Oxygenated fatty acids, 209–210

P

Pantothenic acid, See Vitamin B5
Paraquat, 278–279
Particle size, 438–439
Partition chromatography, carbohydrate analysis by, 299–300
Peak-decay analysis, 14
Peak-fitting methods, 14
Peptides, 306–307
separation, 149–184
Peptidomics, 586–587
Perfluorinated compounds (PFCs), 397–399
Perfluoroalkyl compounds, 339f, 360–372, 362t, 363t
biota, 368–370
human source materials, 370–372
sediments, 367–368
water, 367–368
Perfusion flow rate, analyte recovery determination by, 547–550
Persistent organic pollutants (POPs), 337–388, 339f, 340t
brominated flame retardants, 352–360
brominated cycloalkanes, 356–359
brominated diphenylethers, 353–356
hexabromocyclododecanes, 356–359
tetrabromobisphenol A (4,4’-isopropylidenebis(2,6-dibromophenol), 359–360
chlorinated aromatic compounds, 346–347
perfluoroalkyl compounds, 360–372, 362t, 363t
biota, 368–370
human source materials, 370–372
sediments, 367–368
water, 367–368
pesticides, 347–352
polycyclic aromatic hydrocarbons, 341–346
reference materials, 372–373, 374t–375t
Pesticide-residue analysis (PRA), 319–336
LC–MS analysis, matrix effects in, 324–325
by LC–TOF MS, 331–333
method validation, 325–327
sample analysis, 328–329
sample treatment in, 322–324
specific compounds, individual methods for, 330–331
Pesticides, 339f, 347–352
Pharmaceutical drug development, separation science role in, 432–433
Pharmaceutical industry, high-performance liquid chromatography in, 431–454
chromatographic resolution, increasing, 433–444
column length, 434–438
particle size, 438–439
through selectivity, 439–444
pharmaceutical drug development, separation science role in, 432–433
Pharmaceuticals, 399
Phenyl isocyanate (PIC), 135–136, 136f
Phenyl isothiocyanate (PITC), 135–136, 136f
Phenylthiocarbamyl (PTC) derivatives, 135–136
Phonosphingolipids, 214
Phosarsenoglycosphingolipids, 214
Phosphatidic acid, 211
Phosphatidylcholine, 211
Phosphatidylethanolamine, 211
Phosphatidylinositol, 211
Phosphatidylserine, 211
Phospholipids, See Glycerophospholipids
o-Phosphoserine, 11
Phosphosphingolipids, 214
Photodiode-array detector (DAD), 253
Photoluminescence following electron-transfer (PFET) detection, 565–566
Photoreactors, 51–52
o-Phthalaldehyde (OPA), 137, 574, 576–577
plus chiral thiols, 142
postcolumn fluorescence derivatization with, 133–134, 133f
Phycotoxins, 412
Polar lipids, 205–206
Pollutants, 389–410
general trends in, 391–393
fast chromatography, 391–392
multiresidue methods, 392–393
on-line SPE–LC–MS coupling, 392
LC–MS, target analysis of specific contaminant groups using, 393–403
brominated flame retardants, 393–395
drug abuse, 395–396
endocrine-disrupting compounds, 396–397
hormones, 396–397
nanomaterials, 397
perfluorinated compounds, 397–399
pharmaceuticals, 399
sunscreen agents, 401–403
Polycyclic aromatic hydrocarbons (PAHs), 339f, 341–346
Polyethylene oxide–polypropylene oxide (PEO–PPO) copolymers, 120
Polyketides (PKs), 217, 217f
Polymers, liquid interaction chromatography of, 93–130
barrier methods, 104–105
chromatography at critical conditions, applications of, 99–101
gradient-elution liquid chromatography, 101–104
hyphenated techniques, 107–121
isocratic liquid chromatography, 94–97
liquid-adsorption chromatography, applications of, 98–99
liquid chromatography–Fourier-transform infrared spectroscopy, 111–113
liquid chromatography–mass spectrometry, 115–121
liquid chromatography–nuclear magnetic resonance spectroscopy, 113–115
SEC gradients, 105–107
two-dimensional liquid chromatography, 107–111
Polymer-shielded dye-affinity chromatography, 9–10
Poly(methyl methacrylate) (PMMA), 103, 108–111, 115
Polyterpenes, 216
Polyunsaturated fatty acids (PUFAs), 209
Porous graphitic carbon (PGC) HPLC chromatography, 196
veterinary drug residues analysis by, 461
Positron-emission topography (PET), 542–543
Postcolumn immunodetection, 9
Postcolumn reaction detectors, 49–52
photoreactors, 51–52
Preanalytical specimen handling, in clinical liquid chromatography, 613, 614t
Precision, 65, 68
intermediate, 60t–61t, 62
intraassay, See Repeatability
under run-to-run conditions, 60t–61t
Prenol lipids (PRs), 216
Preparative-scale LC separation, of enantiomers, 83–86
Pressurized-fluid extraction (PFE), See Accelerated-solvent extraction
Principal-component analysis (PCA), 525–528
Process-related impurities (PRIs), 433, 435–436
Procion Blue, 9–10, 10f
Progestogens, 216
Propyl chloroformate (PrCl), 577
Protein liquid chromatography, methods of, 150t, 151–179
affinity chromatography, 166–169
immobilized metal-, 168–173
displacement chromatography, 177–179
hydrophobic-interaction chromatography, 158–161
on hydroxyapatite, 173–174
ion-exchange chromatography, 153–157
on monolithic supports, 175–177
reversed-phase chromatography, 161–166
size-exclusion chromatography, 151–153
Proteins, 306–307
applications in clinical laboratory, 625–627
protein A, 6
protein G, 6
precipitation, 583
separation, 149–184
chromatographic materials for, 150f
tissue, 627–628
Pseudo-affinity chromatography, 168
Pulsed amperometric detectors (PAD), 300–301
Purines, 579–581
4-(1-Pyrene)butyric acid N-hydroxysuccinimide ester, 139–140

Q

Quadrupole–ion trap (QIT), 462
Quadrupole–linear ion trap (QLIT), 462
Quality-by-design (QbD), 64–71
analytical, 64–71, 433
in regulated industries, 71
Quality control, 646–648
Quantification, 646–648
Quantitative affinity chromatography, 11–12
QuECHERS method, 322–323, 460–461
Quinones, 216

R

Radioimmunoassay (RIA), 586–587
Range, 63
Reagent selection, 27–28
chemiluminescence detection, reagents for, 31–35
cyclic derivatives formation, multifunctional reagents for, 46–48
diastereomers formation, reagents for, 43–46, 44t
electrochemical detection, reagents for, 38–40, 39t
fluorescence detection, reagents for, 31–38, 35t–36t
mass-spectrometric detection, reagents for, 40–43, 42t
solid-phase analytical derivatization, 48–49
UV–visible detection, reagents for, 27–31, 30t, 32t–33t
Refractive index (RI), 107, 300–301, 308
Relative peak area (RPA), 530
Relative retention time (RTT), 530
Repeatability, 60t–61t, 62
Reproducibility, 63
Reversed-phase high-performance liquid chromatography (RP-HPLC), 196
for amino acid analysis, 577
for neurotransmitter analysis, 552–553, 554t
for vitamins analysis, 486
Reversed-phase liquid chromatography (RP–LC)
in clinical laboratory, 613–615
compositional analysis by, 306–308, 310
food additives analysis by, 312, 314
in forensic toxicology, 253
inverse, 640
in pharmaceutical industry, 440–442, 444–452
gradient optimization, 447–448
mobile-phase pH optimization, 448–452
organic solvent, 445–447
required method performance, 445
stationary phase, 445–447
temperature optimization, 447–448
protein separation, 158–159, 161–166
for speciation analysis, 640–641
Riboflavin, See Vitamin B2
Risk assessment, analytical method, 70
Robustness, 63
Rodenticides, 281–282
Ruggedness, 60t–61t

S

Saccharolipids (SLs), 216, 217f
Sample(ing), 218–219
analysis, for pesticide-residue analysis, 328–329
extraction, 218–223
preparation, 218–219
for speciation analysis, 635–636
storage and processing, 636–637
treatment, in pesticide-residue analysis, 322–324
Sandwich immunoassay, 9
Saturated fatty acids, 207
Saxitoxin, 425–426
Second-generation anticoagulants, 281–282
Secosteroids, 216
Sediments, 367–368
Selectivity, 60t–61t
high-resolution LC through increased, 439–444
shape, 341–342
Separation
amino acids, See Amino acids separation
bioamines, See Bioamines separation
techniques, for speciation analysis, 637–641
capillary electrophoresis, 641–643
hydrophilic-interaction liquid chromatography, 640–641
iron-exchange chromatography, 639–640
liquid chromatography, 638–641
reversed-phase chromatography, 640–641
size-exclusion chromatography, 639
ultrafiltration chromatography, 638
Shape selectivity, 341–342
Silver-ion liquid chromatography, 231–233
Simulated moving bed (SMB) chromatography, enantiomers separation by, 83–86
SISCAPA (stable-isotope standards and capture by antipeptide antibodies), 625, 627
Size-exclusion chromatography (SEC)
carbohydrate analysis by, 299, 307–308
gradients, 105–107
protein separation, 151–153
for speciation analysis, 639
Solid–liquid extraction (SLE), 297–298
Solid-phase analytical derivatization, 48–49
Solid–phase extraction (SPE), 251–252, 271, 281, 296, 302, 306, 322–323, 460
dispersive, 460–461
Solution stability, 63
Solvent selection, 218–219
Soxhlet extraction, 219–220
Speciation analysis
direct, 637–641
separation techniques, See Separation techniques
nebulizers, use of internal standard–postcolumn dilution, 641–643
sample storage and processing, 636–637
sampling for, 635–636
Specificity, 58
Sphing-4-enine, 213–214
Sphingoid bases derivatives, 213–214
Sphingolipids (SPs), 213–214, 215f
Sphingomyelins, 211, 214
Split-peak method, 14
Stationary phase(s)
chiral, 76–80, 79t, 82, 85
cinchona-alkaloid-bonded, 143
cyclodextrin-bonded, 143
reversed-phase liquid chromatography, 445–447
Stearic acid, 207
Steroids, 216
Sterol lipids (ST), 214–216
Stitched open-tubular (SOT) reactors, 50–51
Strong cation-exchange chromatography (SCEX)
protein separation, 157
Subcritical water extraction (SWE), 297–298
Succinimidyl ferrocenyl propionate (SFP), 143
Sunscreen agents, 401–403
Supercritical fluid chromatography (SFC), enantiomers separation by, 86–87
Supercritical fluid extraction (SFE), 221–222, 297–298
Surface-noncovalent-affinity mass spectrometry (SNA–MS), 15
Sweeteners, 314
Systematic toxicological analysis (STA), 251

T

Tandem mass spectrometry, 42–43
in clinical laboratory, 619
Targeted poisons, 277–282
cyanide, 279–280
diquat, 278–279
glyphosate, 280–281
paraquat, 278–279
rodenticides, 281–282
Taylor dispersion, in microdialysis sampling, 551–552
Temperature-gradient interaction chromatography (TGIC), 104, 107–108, 111
Tetrabromobisphenol A (4,4’-isopropylidenebis(2,6-dibromophenol) (TBBPA), 359–360
Tetrodotoxin (TTX), 415–418, 417t
Therapeutic drug monitoring (TDM), clinical liquid chromatography applications in, 620–621
Thia fatty acids, 210
Thiamin, See Vitamin B1
Thin-layer chromatography (TLC)
detection and quantification in, 226–227
high-performance, 225–226
lipid analysis by, 224–227
two-dimensional, 225–226
Time-of-flight (TOF), 115–116, 261–262, 276–277
analyzers, 236–237
ion-trap, 237–238, 262
orthogonal–accelerated, 239
quadrupole, 236–238, 240, 331
Tissue content, liquid chromatography methods for, 552–556
Tissue proteins, 627–628
α-Tocopherol, 216f
Topology distribution (TD), 107–108
Toxicology testing, in the clinical laboratory, 623–625
Traditional Chinese medicines (TCMs), HPLC analysis of, 519–540
active compounds, on-line HPLC mining of, 531–535
fingerprinting analysis, 523–531
biological, 531–532
chemometric analysis, 525–529
in Chinese Pharmacopoeia 2010, 529–531, 535–536
multidimensional liquid chromatography, 524–525
multicompound quantitation, 521–523
two-dimensional, 526t–527t
Trans fatty acids, 208–209
Transthyretin, 627
Triacylglycerols, 210–211, 210f
Tridecafluoroheptanoic acid (TDFHA), 134–135
Triglycerides, 210–211
Triple quadrupole (QqQ), 240, 461–462
N,N,N’-Tris(carboxymethy)-ethylenediamine, 11
Trueness, 60t–61t
Two-dimensional liquid chromatography
amino acid enantiomers, analysis of, 143–144
of polymers, 107–111
for TCMs analysis, 526t–527t
Two-dimensional thin-layer chromatography, 225–226
Two-site immunometric assay, See Sandwich immunoassay

U

Ubiquinones, 216
Ultrafiltration chromatography, for speciation analysis, 638
Ultra-high-pressure liquid chromatography (UHPLC)–for biogenic amines analysis, 565–567
for fingerprinting analysis, 530
for microdialysis, 553–555
MS/MS, for acetylcholine analysis, 573
for neurotransmitter analysis, 553–555
Orbitrap, for veterinary drug residues analysis, 468, 471
for veterinary drug residues analysis, 461
Ultrasonic nebulizer (USN), 642
UV filters, See Sunscreen agents
UV–Vis detector
UV–visible spectrophotometry, 27–31, 30t
in clinical laboratory, 617
compositional analysis by, 301–302, 308, 310
UV–Vis reagents, derivatization with, 135–137
4-N,N-dimethylaminoazobenzene-4’-sulfonyl chloride (DABS-Cl), 136–137
phenyl isocyanate, 135–136, 136f
phenyl isothiocyanate, 135–136, 136f

V

Validation of liquid chromatographic methods, See Method validation
Venom, 411–414
Veterinary drug residues, 456
European Union, regulatory aspects in, 457–459, 457t
in foods, determination of, by LC–MS chromatography, 455–476, 459f
Virodhamine, 582–583
Vitamin B1, 303, 479–482, 480f
Vitamin B2, 304, 480f, 482–483
Vitamin B3, 304, 480f, 483–484
Vitamin B5, 304, 480f, 484
Vitamin B6, 304–305, 480f, 484–485
Vitamin B8, 480f, 485–486
Vitamin B9, 304, 480f, 486–487
Vitamin B12, 305, 480f, 487–488
Vitamin C, 303, 480f, 488–489
applications in clinical laboratory, 621–622
Vitamins, 301–306
fat-soluble, See Fat-soluble vitamins
liquid chromatography determination of, 477–518
multivitamin methods, 305–306, 497–500
water-soluble, See Water-soluble vitamins

W

Water-soluble vitamins, 303–305
vitamin B1, 303, 479–482
vitamin B2, 304, 482–483
vitamin B3, 304, 483–484
vitamin B5, 304–305, 484–485
vitamin B6, 304–305, 484–485
vitamin B8, 485–486
vitamin B9, 304, 486–487
vitamin B12, 305, 487–488
vitamin C, 303, 488–489
Weak-affinity chromatography (WAC), 2–3
Weak anion exchange (WAX) HPLC chromatography, 193
Wheat-germ agglutinin (WGA), 5–6

X

X-ray absorption near-edge spectroscopy (XANES), 635