Robin Whelpton - Fundamentals of Analytical Toxicology

4 Chapter 4Figure 4.1 Summary of the steps that may be involved in an analysisFigure 4.2 Microextraction procedure flow-diagrams: (a) prior to GC; (b) pri...Figure 4.3 Extraction of imipramine and three metabolites from buffers of va...Figure 4.4 Schematic diagram of a solid phase extraction procedureFigure 4.5 HybridSPE-Phospholipid technologyFigure 4.6 Solid phase microextraction: (a) spring-loaded solid probe coated...Figure 4.7 Equilibration time profile for SPME of lidocaine from plasma afte...Figure 4.8 Schematic of modes of liquid phase microextraction: (a) single dr...Figure 4.9 Supercritical fluid extraction. (a) Phase diagram for a fluid. (b...Figure 4.10 Schematic diagram of apparatus for accelerated solvent extractio...Figure 4.11 Diagrammatic representation of equilibrium dialysis. (a) Equilib...

5 Chapter 5Figure 5.1 The basic components of a single-beam spectrophotometerFigure 5.2 Diagram of a typical optical-null double-beam spectrophotometerFigure 5.3 Diagram of a linear diode array detectorFigure 5.4 Measurement of carboxyhaemoglobin (note the wavelength expansion ...Figure 5.5 Conway microdiffusion. (a) Apparatus. (b) Qualitative detection o...Figure 5.6 Diagram of a double-grating spectrophotofluorimeter (based on the...Figure 5.7 Excitation and emission spectra of quinine (1 mg L –1) in de...Figure 5.8 Some compounds that exhibit natural fluorescenceFigure 5.9 Chemiluminescent reaction of luminol with hydrogen peroxideFigure 5.10 Hydrogen peroxide oxidation of TCPOFigure 5.11 A simple luminometerFigure 5.12 Schematic diagram of laser Raman spectroscopy

6 Chapter 6Figure 6.1 Preparation of immunogen for chlorpromazine radioimmunoassayFigure 6.2 Directing antibody formation for a class-selective and an analyte...Figure 6.3 Principle of competitive bindingFigure 6.4 Reaction of tetramethylbenzidine with hydrogen peroxide in the pr...Figure 6.5 Comparison of (a) antigen-labelled and (b) antibody-labelled ELIS...Figure 6.6 Representation of sandwich ELISA microplate well after its second...Figure 6.7 Principle of enzyme-multiplied immunoassay technique (a) without ...Figure 6.8 Principle of fluorescence polarization immunoassay: (a) without a...Figure 6.9 Principle of cloned enzyme donor immunoassay. (a) No added drug a...Figure 6.10 Different modes of measurement for turbidimetric assaysFigure 6.11 RIA calibration graphs showing original data (a) transformed to ...Figure 6.12 Alcohol dehydrogenase catalyzed oxidation of ethanolFigure 6.13 Oxidation of ethanol catalyzed by alcohol oxidaseFigure 6.14 Reaction of Ellman's reagent with thiols

7 Chapter 7Figure 7.1 Elution chromatography: retention timeFigure 7.2 Schematic representation of a fractionating column showing the co...Figure 7.3 Chromatographic efficiency: (a) measurement of H; (b) effect of m...Figure 7.4 Effect of particle size and linear velocity on H using ∼2 μm size...Figure 7.5 Kinetic plots ( t M/ N 2against plate number) for two packing materi...Figure 7.6 Effect of efficiency on resolution of A and B. Values calculated ...Figure 7.7 Measurement of peak asymmetry

8 Chapter 8Figure 8.1 Thin-layer chromatography: schematic and calculation of R fvalues...Figure 8.2 Comparison of the migration of the solvent front in saturated and...Figure 8.3 Example of differential visualization of a TLC plate (Flanagan et ...Figure 8.4 Hydrolysis of benzodiazepines and dealkylation of N -alkylbenzophe...Figure 8.5 Two modes of forced-flow planar chromatography (Bryston & Papilla...

9 Chapter 9Figure 9.1 Block diagram of a gas chromatographFigure 9.2 Split/splitless injector for gas chromatographyFigure 9.3 Schematic of (a) GC thermal desorption unit; (b) modes of useFigure 9.4 Schematic diagram of a GC thermal conductivity detectorFigure 9.5 Schematic diagram of a GC flame ionization detectorFigure 9.6 Schematic diagrams of (a) nitrogen–phosphorus detector and (b) el...Figure 9.7 Schematic diagram of a pulsed discharge helium ionization detecto...Figure 9.8 Schematic diagram of a GC vacuum UV detectorFigure 9.9 Structures of polysiloxane and polyethylene glycol stationary pha...Figure 9.10 Schematic of a fused silica capillary GC columnFigure 9.11 Schematic diagram of 2D-GCFigure 9.12 GC headspace vialFigure 9.13 Examples of chemically bonded chiral phases. (a) β -CD bonde...Figure 9.14 Extracted negative ion chromatograms (GC-MS) of R -/ S -enantiomers...

10 Chapter 10Figure 10.1 Schematic diagram of a dual pump gradient LC system with high-pr...Figure 10.2 Structure of polyoxy-1,4-phenyleneoxy-1,4-phenylenecarbonyl-1,4-...Figure 10.3 LC pump head during a filling strokeFigure 10.4 Six-port LC injection valve showing (a) load and (b) inject posi...Figure 10.5 Schematic diagram of UV/visible detector flow cell for LCFigure 10.6 Schematic diagram of a combined fluorescence/UV detector cell fo...Figure 10.7 Simplified designs of LC-ED cells. (a) Thin-layer cell, (b) Wall...Figure 10.8 Schematic diagram of chemiluminescent nitrogen detector (Nussbau...Figure 10.9 Schematic diagram of a charged aerosol detector (Magnusson et al Figure 10.10 Arrangement for post-column reagent addition in liquid chromato...Figure 10.11 Example of a bridged ethylsiloxane/silica hybrid LC packingFigure 10.12 Schematic diagram of affinity chromatographyFigure 10.13 Typical calibration curve for size exclusion chromatographyFigure 10.14 Representation of chiral recognition. The structure with three-...Figure 10.15 Analysis of 3,5-dinitrobenzamide derivatives of (a) amfetamine,...Figure 10.16 Derivatization of racemic amfetamine to provide points of inter...Figure 10.17 Effect of the nature of the column packing on the liquid chroma...Figure 10.18 Liquid chromatography of lidocaine using Waters Spherisorb S5 S...

11 Chapter 11Figure 11.1 (a) Phase diagram for carbon dioxide. (b) Effect of addition of ...Figure 11.2 Schematic diagram of a packed column supercritical fluid chromat...Figure 11.3 Schematic diagram of supercritical fluid chromatography pressure...Figure 11.4 Resolution of warfarin enantiomers on a CHIRALPAK AD column in (...Figure 11.5 Chemical formulae of ketamine and selected metabolitesFigure 11.6 Supercritical fluid chromatography of JWH-073. (a) Blank urine; ...

12 Chapter 12Figure 12.1 Schematic diagram of the arrangement for capillary electrophores...Figure 12.2 Diagram showing how electro-osmotic flow carries analytes to the...Figure 12.3 Principle of micellar electrokinetic capillary chromatographyFigure 12.4 Elution time window for non-ionized species in MEKCFigure 12.5 Micellar electrokinetic capillary chromatography of some misused...Figure 12.6 Sample electropherograms of (a) blank EBC, (b) an EBC sample spi...

13 Chapter 13Figure 13.1 Schematic diagram of a double sector mass spectrometerFigure 13.2 Schematic diagram of a quadrupole mass spectrometerFigure 13.3 Schematic diagram of an ion trap quadrupole mass spectrometerFigure 13.4 Schematic diagram of a triple-quadrupole mass spectrometer (Tand...Figure 13.5 Schematic diagram of Q3 in a QTrap system. (a) Quadrupole and ex...Figure 13.6 Schematic diagram of a common time-of-flight tandem MS (QTOF) (r...Figure 13.7 Schematic diagram of an orbitrap tandem mass spectrometer (Q-Exa...Figure 13.8 Schematic side-view of an electron ionization sourceFigure 13.9 Schematic diagram of a typical GC-C-IRMS Instrument: configured ...Figure 13.10 Ion suppression. Response after injection of (i) an extract of ...Figure 13.12 Electrospray ionization: schematic of the mechanism of ion form...Figure 13.11 Schematic of an electrospray ionization interfaceFigure 13.13 Schematic of the components of an atmospheric pressure chemical...Figure 13.14 Atmospheric pressure chemical ionization: explanation of corona...Figure 13.15 Schematic diagram of an APPI interfaceFigure 13.16 Analytical figures of merit versus analytical throughput of chr...Figure 13.17 (a) Scheme of FIA-MS with LC autosamplers. (b). Diagram of a FI...Figure 13.18 Schematic diagrams of (a) DART ionization and (b) ESI or EASI s...Figure 13.19 Analysis of a dried blood spot by paper spray-MS (Reprinted fro...Figure 13.20 Schematic diagram of a laser diode thermal desorption sourceFigure 13.21 Principle of matrix assisted laser desorption/ionization mass s...Figure 13.22 Typical MALDI applications in forensic toxicology: (a) high-thr...Figure 13.23 Typical GC-MS total ion chromatogram of a methanolic solution c...Figure 13.24 Mass spectra of citalopram ( M r324.4) and clomipramine ( M r314....Figure 13.25 EI mass spectra of amfetamine ( M r135.2) and metamfetamine ( M r...Figure 13.26 EI mass spectra of the 4-carboxyhexafluorobutyryl (4-CHFB) deri...Figure 13.27 Problems associated with deuterated internal standards. (a) Sep...Figure 13.28 Isotopic internal calibration in LC-MS/MS: plasma clozapine and...Figure 13.29 MALDI-MS/MS images of (a) longitudinal sectioned drug user hair...