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Summary
Summary
This unique collection contains data obtained from clinical samples over the course of more than 20 years. It encompasses 7500 potentially harmful substances, from simple analgesics to designer drugs, and from pesticides to chemical warfare agents. Since these substances are often broken down in the human body, metabolites are also included, so as to allow quick and unambiguous identification of the mother substance. The 3rd edition gives all spectra in order of their molecular mass, since this has become the prime benchmark criterion for the identification of unknown substances.
Reviews 1
Choice Review
By any definition, this set of mass spectra and gas chromatography (GC) data is a monumental work. Its 4,370 mass spectra cover 1,500 drugs, 800 pesticides and pollutants, and 2,000 metabolites. The spectra are in bar graph form with m/z ratios of major peaks shown. Each spectrum is accompanied by a wealth of data such as structure, synonyms, Chemical Abstracts Service (CAS) cross-list, GC retention indexes, and pharmacological category. An extensive methods section includes detailed instructions on extraction, derivatization, and cleaning up biological samples, and information on mass spectral interpretation and instrumentation. Numerous tables cross-list entries by a number of criteria, including name, pharmacological category, and retention index. Separate tables of potential poisons are arranged by molecular mass, name category, and CAS cross-index. Volume 2 contains mass spectra of substances whose fragments are between m/z 4 and 221; Volume 3 contains mass spectra of m/z up to 777. A supplement to the collection is available with computer-readable spectra. Graduate through professional. J. A. Siegel; Michigan State University
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 |