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INDEX

485 486 INDEX

CITAC, 13, 24 response factors, relative, 301 Clathrate, 101 selectivity 279, 283᎐284 Clausius-Clapeyron equation, 171 signal, 291᎐295 Code of Federal RegulationsŽ. CFR , 9, 11 time constant of, 287᎐290 Part 11, 30 Dialysis, 411᎐412 Column: Diastereomer separations, 445᎐446 microbore, 240 Development of methods, 4, 248᎐250 open tubularŽ. OT , 143, 153᎐157 Diffusion, 77, 370 packed, 68᎐74 Diffusion coefficient, 77 wide-bore, 157 Dispersion forces, 98 Column selectivity, see Separation factor Dispersivity, 90, 109, 135 Comparisons: Displacement , 43 CEC and CZE, 382 , 47᎐49, 106, 392᎐393. gases and liquids, 118᎐119 Drift, 286 GC and LC, 117᎐124 Dual detectorsŽ. dual channel GC , 359 linear flow and electroosmotic flow, 375 Dwell volume and time, 257᎐258 peak height and peak area, 296᎐297 peaks and bands, 135᎐136 Eddy diffusion, 76 retardation factors, RF and R, 136᎐139 Effective plate number, 54 Compressibility factor, 120᎐121 Electrochemical detectors in LC, 247 Corrected retention volumeŽ. time , 120 Electron capture detectorŽ. ECD , 164᎐165 Countercurrent chromatography, 454᎐455 Electron impact, 311 Craig countercurrent extraction apparatus, 397 Electronic pressure control, 150 point data, 126 Electrophoresis: Critical micellar concentration, 379 capillary electrophoresis, 372᎐380 Cryogenic GC, 176 principles of, 366᎐371 Current Good Manufacturing Practice zone electrophoresis, 371᎐372 Ž.CGMP . See Good Manufacturing Electroosmosis and electroosmotic flow, 370, PracticeŽ. GMP 373᎐375 Curves: Electrospray ionization, 316᎐318 calibration, 292, 295, 302, 304 Eluotropic series, 199 vanDeemter, 82, 83, 86, 87, 89, 90 Elution, gradient, see Gradient elution Cyclodextrin, 448 Elution chromatography, 43 CZE, see capillary electrophoresis End capping, 202 Environmental Protection Agency, EPA, 11, Data, acquisition of, 296᎐299 14 Data systemŽ. s : Equations, summary table of, 63 ChromatographyŽ. CDS , 296 Equivalent columnŽ. s in HPLC, 207 LIMS, 296 Evaporative light scattering detectorŽ. ELSD , Dead volume, see hold-up volume 247᎐248 DEGS, 170 Extended , 80 Densitometry, in TLC, 345 External standard, 301᎐303 Derivatization, 412᎐417 Extra-column zone broadening, 242᎐243 Detection limitŽ. s , 27, 476. See also Detectivity Extraction, 390᎐411 Detectivity, 292, 293᎐294 Detectors, 278᎐296 Flame ionization detectorŽ. FID , 157᎐161 cell volume of, 290᎐291 Flash chromatography, 265 characteristics of, 285᎐296 Fast GC, 176, 177 classification of, 278᎐284 Fast LC, 240 minimum detectability, see Limit of FDA, see Food and Drug Administration detection LOD Federal Register, 9, 22 GC, 157᎐165 Field flow fractionation, 455 HPLC, 243᎐248 Flow, measurement of in GC, 121 linear range, 292, 294 Flow resistance parameter, 122, 268 noise, 285᎐287 Fluorescence detector, 247 INDEX 487

Food and Drug AdministrationŽ. FDA , 2, 6᎐11 Hydrophobic interaction chromatography FR, see Federal Register Ž.HIC , 209᎐210, 442᎐443 Frontal analysis, 44 Hydrophilic interaction chromatography Fronting, see Peak, shape of Ž.HILIC , 261

GAMP, see Good automated manufacturing IC, see practice ICH, see International Conference on Gas compressibility factor, 119᎐121 Harmonization, Gas-liquid chromatographyŽ. GLC , 143᎐144 Ideal solution, 104 Gas-solid chromatographyŽ. GSC 100, 101, Inclusion compounds, 101 143᎐144, 167 Induction forces, 98 Gaussian distribution, see Normal distribution Injection port, GC, 150, 165᎐166 GCrFTIR, 327 Injection valve, 239 GCrMS, 323 Installation qualificationŽ. IQ , 29 Gel filtration, see Size exclusion Instrument qualification, see Qualification of chromatography instruments Gel permeation, see Size exclusion Inorganic GC, 178 chromatography Integration of peaks, 297᎐299 General Notices, 20 Internal standard, 303, 323 GLP,see Good Laboratory Practice Internal surface reversed phaseŽ. ISRP LC, GMP, see Good Manufacturing Practice 211᎐212 Golay equation, 81 International Conference on Harmonization Good automated manufacturing practice Ž.ICH , 7, 11, 21᎐22 Ž.GAMP , 29 glossary of terms, 475᎐477 Good guidance practicesŽ. GGP , 10 International Organization for Good laboratory practiceŽ. GLP , 7 Standardization,Ž. ISO , 16 Good Manufacturing PracticeŽ. GMP , 2, 7, 9 International Union of Pure and Applied Gradient elution, 188᎐190, 199, 237, 256᎐258, Chemistry,Ž. IUPAC , 13, 17 383 Internet web sites, 13, 34, 472᎐473 Guidance documents, 10 Inverse GC, 178 GXP, 7, 10 Ion chromatography, 220᎐225 Ion exchange chromatography, 214᎐225 HorHETP, 55. See see Dispersivity and Plate Ion interaction chromatographyŽ. IIC , 207᎐211 height Ion pair chromatography, see Ion interaction Headspace analysis, 410᎐411 chromatographyŽ. IIC Henrys Law, 102 Ion sources, MS, 311᎐318 High performance liquid chromatography, Ion trap analyzer, MS, 319 HPLC, 186᎐188 Ionic mobility, 367 column diameter, 240᎐242 ISO, see International Organization for column efficiency, 268 Standardization column equivalency, 207 Isocratic LC, definition of, 188 column evaluation, 268᎐269 Isothermal chromatography, 173 detectors, 243᎐248 Isotherms, sorption, 94 instrumentation, 234᎐249 IUPAC, 13, 17 pumps, 234᎐237 Nomenclature, 45 temperature control, 242 troubleshooting, 259᎐261 Keesom forces, 98 High performance TLCŽ. HPTLC , 336᎐337 Kinetics of chromatography, 67, 75᎐88 High pressure LC, 186 Kovats retention index, 144᎐146 Hildebrand’s solubility parameter, 104᎐105 Knox equation plot, 89᎐90 History of chromatography, 37, 141 Hold-up volume, 48 Lab-on-a-chip, 455 Homologous series plots, 145 Laboratory Information Management Systems HPLC, see High performance LC Ž.LIMS , 296 Hydrogen bonding, 99 Langmuir isotherm, 95 488 INDEX

Large volume injection, GC, 178 Molecular weight determination by SEC, LCrFTIR, 327 232᎐234 LCrMS, 324᎐326 Monolithic columns, 71᎐72, 191, 212᎐213 LCrNMR, 327 Multidimensional chromatography, 423᎐432 Ligand exchange chromatography, 225 GCrGC, 425᎐427 Limit of detectionŽ. LOD , 29, 293᎐294 LCrGC, 427᎐431 Limit of quantitationŽ. LOQ , 294 LCrLC, 431᎐432 LIMS, see Laboratory information TLC, 347 management systems Multipath term in rate equation, 76 Linearity of detectors, 294᎐295, 477 Linear dynamic range, 294᎐295, 477 National Formulary, 19 Liquid chromatographyŽ. LC . See also High National Institute of Standards and performance liquid chromatography TechnologyŽ. NIST , 5 Ž.HPLC NDA, see New drug application low pressure, 185, 186 Net retention volume, 121 normal phase, 184, 194 New drug applicationŽ. NDA , 7 planar, see thin layer chromatographyŽ. TLC NIST, see National Institute of Standards and preparative, 262᎐266 Technology reversed phase, 184, 248᎐258 Nitrogen phosphorous detector, 164 Liquid-liquid extractionŽ. LLE , 393᎐402 NoiseŽ. detector , 285᎐287 Liquid-liquid microextraction, 398 Nomenclature, see IUPAC nomenclature Liquid phase, see Stationary phase Non-retained soluteŽ. peak , 47᎐48 Liquid-solid chromatographyŽ. LSC , 194᎐198 Non-volatile samples, 468᎐471 Liquid-solid extraction, 402᎐404 Normal distribution, 51᎐52 London forces, 98 Normal phase LCŽ. NPLC , 184, 194 Longitudinal molecular diffusion, 77 NTIS, 12 Low pressure LC, 185, 186 Number of theoretical plates, see Plate number

Martin equation, 343 Open tubularŽ. OT columns, see Mass spectroscopyŽ. MS and MSD , 310᎐324 Column, open tubularŽ. OT analyzers, 318᎐321 Operational qualificationŽ. OQ , 30 ion sources, 311᎐318 Optimization of separations, 112᎐115 Mass transfer, 78᎐79 Orientation forces, 98 MDQ, see Limit of detectionŽ. LOD Overlapping resolution mapping, 249᎐254 Method development, 249᎐259 computer methods, 258 Packed columns, 68᎐74 Method translation, 176 nature of, 73᎐74 Method validation, see Validation PAGE, 371᎐372 Micellar LC, 267 , 331᎐332 Micellar electrokinetic chromatography Particle beam, 314᎐315 Ž.MEKC , 379 Particle size, effect on efficiency, 87 Microbore columns in LC, 240 Partition, 44 Microfluidic devices, 455 Partition coefficient, 105. See also Distribution Microliter syringe, see Syringe constant ␮TAS, 455 Partition ratio, see Retention factor Minimum detectable quantityŽ. MDQ or Peak: Minimum detection limit, see Limit of definition of, 45, 52 Detection shape of, 55, 94 Mobile phase: symmetry of, 55᎐57 GC, see Carrier gas Peak capacity, 60 LC, 191᎐194. See also BufferŽ. s in HPLC Peak fronting, 55 Mobility, see Ionic mobility Peak height vs. peak area, 296 Molecular diffusion, see Diffusion Peak parking, 281 Molecular imprint polymersŽ. MIP , 407, 437 Peak tailing, 55 Molecular sieves, 100 Peak width, 52, 297 INDEX 489

Pellicular supports, 191 Restricted access mediaŽ. RAM , 210, 410, 434 Performance qualification, 30 for columnar kit for, 267 chromatography, R,49᎐51 Permeability, 121᎐122 Retardation factor for planar chromatography, ᎐ ᎐ Phase selection diagrams, 254 255 RF , 136 138 Phase volume ratio, 49, 155 Retention gap, 157 Photodiode array, see Diode array detector, Retention index of Kovats, 144᎐146 PinkertonŽ. ISRP columns, 210᎐211 Retention factor, 49 Plate height, 55, 90 Retention time, 47 Plate number, 53 Retention time locking, 176 Plate theory, 75, 398 Retention volume, 46᎐49 Polarity index, 106᎐107 adjusted, 48 Pore size of LC supports, 68᎐70 corrected, 120 Porosity, 74 net, 121 Precision, 27, 295᎐296, 476 specific, 143 Preparative scale: Reversed phase LC, 184, 249᎐259 LC, 262᎐267 Robustness, 295, 477 TLC, 347 RohrschneiderrMcReynolds constants, Pressure correction factor, 119᎐121 146᎐147, 192 Pressure equivalences, 118, 150 Ruggedness, 295᎐296 Prisma, 338 Programmed temperature GCŽ. PTGC , Sample size, maximum for preparative LC, 172᎐176 266 Programmed temperature vaporization, 177 Sampling valve, 239 Proteins, peptides, and proteomics, 438᎐440 Selected ion monitoringŽ. SIM , 322 Pseudophase LC, 267 Selectivity, detector, 279, 283᎐284. See also Pumps for LC, 234᎐237 Separation factor Pyrolysis GC, 178 SensitivityŽ. detector , 291 Separation, definition of, 39 Quadrupole analyzer, MS, 319 Separation factor, 62, 355 Qualification of instruments, 4, 9, 29 Separation impedance, 268 Quality assurancercontrol, 3 Separation number, 61 Quantitative analysis, 299᎐306 Septum, 150, 151 Quantitation limit, definition of, 477 Sieving, molecular sieves, 100. See also Quarter-peak width, 52 Size exclusion chromatography Signal-to-noise ratioŽ. SrN,286 Range, see Linear dynamic range Significant temperature, 176 Raoults Law, 142 Silanization of solid supports, 73 Rate equations, comparisons of, 79᎐82, 84᎐88 Silica: Rate theory, 75᎐91 surface of, 72 Ratiograms, 359᎐362 types of, 72, 201, 204 Reduced parameters, 88᎐90, 134 Silicone polymer stationary phases, 169᎐170 Reference standards, 6, 17᎐19, 299᎐300 Simulated distillation,179 Refractive indexŽ. RI detector, 246 Size exclusion chromatography, 100, 226᎐234 Regular solution, 104 Snyder’s solvent parameter, 104᎐107, 192᎐195 Relative response factors. See Response Soap chromatography, 208, 267 factors Solid adsorbentsŽ. stationary phases , 16 Relative retention, 355 Solid phase extractionŽ. SPE , 405᎐407 Repeatability, see Precision Solid phase microextractionŽ. SPME , 407᎐410 Reproducibility, see Precision, Solid support, 67 Research and developmentŽ. R&D , 3 Solubility parameter of Hildebrand, 104, 105 Resolution, 58᎐59 Solvophobic theory, 203 in MS, 321 Sorption, see Absorption; Adsorption Response factorsŽ. detector , 301 Sorption isotherms, 94 Response time, 287 Specificity, 475 490 INDEX

Split injection, 150᎐152 TLC, see Thin layer chromatography Splitless injection, 151᎐153 Total ion chromatogramŽ. TIC , 322 Splitter, inlet for GC, 150᎐152 Trennzahl number, 61 SRM, see Reference standards TrifluoroacetateŽ. TFA , 325 Standard addition, 304᎐305 Troubleshooting, HPLC, 259᎐261 Standard deviationŽ. quarter-zone width , Troutons rule, 174 51᎐53 Tswett, 37 Standard operating procedureŽ. SOP , 27 Two-column plots, 355᎐357 Standardization, 17᎐19 Standards, chemical, see Reference standards Ultraviolet absorption detectorŽ. UV , 244᎐246 Stationary phase: Unified chromatography, 37, 125 configuration of, 67᎐74 United States PharmacopeiaŽ. USP , 10, 13, in GC, 85, 166᎐167, 168᎐170 19᎐21 in LC, 87, 190. See also Bonded phases general notices, 20 in TLC, 335᎐338 reference standards, 20 Statistical moments, 54 relationship to the FDA, 10 Stir-bar sorptive extraction, 410 Ž. Supercritical fluid chromatography SFC , 37, Validation of methods, 4, 7, 9, 10, 18, 24᎐29, ᎐ 124 134 295 ᎐ Supercritical fluids, 124 129 Valve, sampling, 238᎐239 Ž. ᎐ Supercritical fluid extraction SFE , 404 405 Van Deemter equation, 75᎐79 ᎐ Surface deactivation, 72 73, 201 Van Deemter plots, 83 Syringe, 150, 151 Van der Walls forces, 97᎐99 System peaks, 246 Velocity: Ž. System suitability SS , 21, 28, 305 average linear, of mobile phase, 49, 120 of solute, 49 ᎐ Tailing factor, 55 57 reduced, see Reduced parameters Tandem MS, 322 Viscosity of water mixtures, 238 TCD, see Thermal conductivity detector Void volume, see Hold-up volume ᎐ Temperature, effect in GC, 170 176 Volatile samples, 468 Temperature programming, see Programmed Volume: temperature GC hold-up, 48 Theoretical plate, see Plate number retention, 47 Ž.᎐ Thermal conductivity detector TCD , 161 163 VTR2AP methodology, 27 Thermodynamics of zone migration, 111 Thermospray ionization, 315᎐316 Wall-coated OT columns , GC, 85, 143, 144, Thin layer chromatographyŽ. TLC , 333᎐350 154᎐157, 166 classification of, 343 Water, GC separation of, 167 instrumental, 341᎐350 manual, 333᎐341 OPLC, 344᎐345 Xylene isomers, separation of, 103 Threshold, 298 Time, retention, see Retention time Zirconia bonded phases, 213 Time constantŽ. detector , 287᎐290 Zone, definition of, 135 Time of flightŽ. TOF analyzer, MS, 319 Zwitterion, 368