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This paper reviews procedures for the detection or quantification of drugs, pesticides, pollutants, and/or their metabolites relevant to clinical and forensic toxicology, doping control, or biomonitoring using gas chromatography–mass spectrometry with negative ion chemical ionization (GC-MS-NICI). Papers written in English between 1995 and 2000 are reviewed. Procedures are included for the analysis of the following halogen-containing or derivatizable compounds in common biosamples, such as whole blood, plasma, or urine, and in alternative matrices such as sweat, hair, bone, or muscle samples of humans or rats: benzodiazepines, cannabinoids, opioids, acetylsalicylic acid, angiotensin-converting enzyme inhibitors, ketoprofen, methylphenidate enantiomers, tegafur, zacopride, anabolic steroids, chlorophenols, chlorpyrifos, hexachlorocyclohexanes, organochlorines, and polychlorinated biphenyls. The principal information on each procedure is summarized in three tables to facilitate the selection of a method suitable for a specific analytic problem.