Table of Contents

Volume 1 (Methods, Tables). 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.

About the Author

Karl Pfleger was appointed head of the Department of Toxicology at the Saarland University in Homburg/Saar, Germany, in 1967. In the late 1970s he developed, together with his PhD student Hans H. Maurer, novel analysis procedures for identification and Quantification of drugs, poisons and their metabolites in body samples. they introduced mass spectrometry as the gold standard into clinical and forensic toxicology. In 1985, they published the first edition of their unique handbook of GC and MS data together with Armin A. Weber (left), who was and is responsible for all technical and software developments, including the mass spectral database that was developed from the printed collection. In 1987, Karl Pfleger received the Jean-Servais Stas Medal of the Gesellschaft fur Toxikologische und Forensische Chemie (GTFCh). In 1992, Karl Pfleger retired and Hans H. Maurer became his successor as professor and head of the department. His main areas of research are analytical toxicology (GC-MS, LC-MS) and metabolism of xenobiotics. He has published over 130 original papers and 20 invited reviews. He has received several scientific awards, including the Young Investigator Award of the Homburg Medical Faculty in 1983, the Irving Sunshine Award for Outstanding Contributions to Clinical Toxicology of the International Association of Therapeutic Drug Monitoring and Clinical Toxicology (IATDMCT) in 1997, the Alan Curry Lifetime Achievement Award of The International Association of Forensic Toxicologists (TIAFT) for Outstanding Contributions to Forensic Toxicology in 2003, and the Doctor Honoris causa title of the University of Ghent in 2007. He is the current President of IATDMCT (since 2007), Councillor of TIAFT (since 2005) and treasurer of GTFCh (since 1987).

Reviews

Praise for the previous edition: "An invaluable source of reference for any environmental, toxicological or analytical laboratory." (Rapid Communications in MS) "The excellent organization of the information facilitates their everyday use. Highly recommended." (Environmental Science and Pollution Research) "The modern toxicological laboratory can ill afford to be without this unique work." (Veterinary Human Toxicology)