 Mass Spectral and GC Data of Drugs, Poisons, Pesticides, Pollutants and Their Metabolites, 3rd Edition, 2 Volumes
ISBN: 978-3-527-31538-3
Hardcover
1452 pages
July 2007
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Methods.
1 Introduction.
2 Experimental Section.
2.1 Origin and choice of samples.
2.2 Sample preparation.
2.2.1 Standard extraction procedures.
2.2.1.1 Standard liquid-liquid extraction (LLE) for plasma, urine or gastric contents (P, U, G).
2.2.1.2 STA procedure (hydrolysis, extraction and microwave-assisted acetylation) for urine (U+UHYAC).
2.2.1.3 Extraction of urine after cleavage of conjugates by glucuronidase and arylsulfatase (UGLUC).
2.2.1.4 Extractive methylation procedure for urine or plasma (UME, PME).
2.2.1.5 Solid-phase extraction for plasma or urine (PSPE, USPE).
2.2.1.6 LLE of plasma for determination of drugs for brain death diagnosis.
2.2.1.7 Extraction of ethylene glycol and other glycols from plasma or urine followed by microwave-assisted pivalylation (PEGPIV or UEGPIV).
2.2.2 Derivatization procedures.
2.2.2.1 Acetylation (AC).
2.2.2.2 Methylation (ME).
2.2.2.3 Ethylation (ET).
2.2.2.4 tert.-Butyldimethylsilylation (TBDMS).
2.2.2.5 Trimethylsilylation (TMS).
2.2.2.6 Trimethylsilylation followed by trifluoroacetylation (TMSTFA).
2.2.2.7 Trifluoroacetylation (TFA).
2.2.2.8 Pentafluoropropionylation (PFP).
2.2.2.9 Pentafluoropropylation (PFPOL).
2.2.2.10 Heptafluorobutyrylation (HFB).
2.2.2.11 Pivalylation (PIV).
2.2.2.12 Heptafluorobutyrylprolylation (HFBP).
2.3 GC-MS Apparatus.
2.3.1 Apparatus and operation conditions.
2.3.2 Quality assurance of the apparatus performance.
2.4 Determination of retention indices.
2.5 Systematic toxicological analysis (STA) of several classes of drugs and their metabolites by GC-MS.
2.5.1 Screening for 200 drugs in blood plasma after LLE.
2.5.2 Screening for most of the basic and neutral drugs in urine after acid hydrolysis, LLE and acetylation.
2.5.3 Systematic toxicological analysis procedures for the detection of acidic drugs and/or their metabolites.
2.5.4 General screening procedure for zwitterionic compounds after SPE and silylation.
2.6 Application of the electronic version of this handbook.
2.7 Quantitative determination.
3 Correlation between Structure and Fragmentation.
3.1 Principle of electron-ionization mass spectrometry (EI-MS).
3.2 Correlation between fundamental structures or side chains and fragment ions.
4 Formation of Artifacts.
4.1 Artifacts formed by oxidation during extraction with diethyl ether.
4.1.1 N-Oxidation of tertiary amines.
4.1.2 S-Oxidation of phenothiazines.
4.2 Artifacts formed by thermolysis during GC (GC artifact).
4.2.1 Decarboxylation of carboxylic acids.
4.2.2 Cope elimination of N-oxides (-(CH3)2NOH, -(C2H5)2NOH, -C6H14N2O2).
4.2.3 Rearrangement of bis-deethyl flurazepam (-H2O).
4.2.4 Elimination of various residues.
4.2.5 Methylation of carboxylic acids in methanol ((ME), ME in methanol).
4.2.6 Formation of formaldehyde adducts using methanol as solvent (GC artifact in methanol).
4.3 Artifacts formed by thermolysis during GC and during acid hydrolysis (GC artifact, HY artifact).
4.3.1 Dehydration of alcohols (-H2O).
4.3.2 Decarbamoylation of carbamates.
4.3.3 Cleavage of morazone to phenmetrazine.
4.4 Artifacts formed during acid hydrolysis.
4.4.1 Cleavage of the ether bridge in beta-blockers and alkanolamine antihistamines (HY).
4.4.2 Cleavage of 1,4-benzodiazepines to aminobenzoyl derivatives (HY).
4.4.3 Cleavage and rearrangement of N-demethyl metabolites of clobazam to benzimidazole derivatives (HY).
4.4.4 Cleavage and rearrangement of bis-deethyl flurazepam (HY -H2O).
4.4.5 Cleavage and rearrangement of tetrazepam and its metabolites.
4.4.6 Dealkylation of ethylenediamine antihistamines (HY).
4.4.7 Hydration of a double bond (+H2O).
5 Table of Atomic Masses.
6 Abbreviations.
7 References.
Tables.
8 Table of Compounds in Order of Names.
8.1 Explanatory notes.
8.2 Table of compounds in order of names.
9 Table of Compounds in Order of Categories.
9.1 Explanatory notes.
9.2 Table of compounds in order of categories.
Volume 2 (Mass Spectra).
1 Explanatory Notes.
1.1 Arrangement of spectra.
1.2 Lay-out of spectra.
2 Abbreviations.
3 Compound Index.
Mass Spectra.
