This paper describes analytical methods using high-performance liquid chromatography and gas chromatography-mass spectrometry (GC-MS) for the isolation of the nonsteroidal anti-inflammatory drug, ketorolac. The drug is isolated from postmortem blood using a batched solid-phase extraction method on Amberlite XAD-2 resin. Derivatization of ketorolac using diazopropane was necessary prior to GC-MS analysis. The methods were applied in the investigation of a death occurring shortly after the administration of an intramuscular injection of ketorolac tromethamine. Death was attributed to an adverse reaction to the drug, resulting in anaphylaxis and cardiac arrest.

Quantitative recovery of drugs from biological samples is important when a response is to be related to the amount of drug present in a tissue sample. Morphine is one drug of interest in this regard because of its widespread use and its chemical peculiarities. Its relatively low dosage, amphoteric nature, and metabolism to a water-soluble product, 3-morphine monoglucuronide [1,2], make morphine relatively difficult to analyze in biological samples. Most quantitative analytical schemes of analysis require that the glucuronide be cleaved to free morphine for extraction into an organic solvent. Acid hydrolysis [3] and enzymatic cleavage [4] are the most popular methods for freeing the morphine. We report here a study of the recoveries of radioactively tagged morphine from biological samples of morphine-treated dogs by using hydrolysis and solvent extraction. It is possible to recover more than 90% of the morphine contained in a sample with acid hydrolysis and about 80% with enzymatic cleavage.

Basic drugs are extracted from urine or drug preparations at pH 9.5-11 into cyclohexane or heptane containing a small amount (ca. 0.1%) of benzene. The presence of the benzene introduces fine structure in the ultraviolet spectra of compounds that ordinarily give qualitatively similar spectra. This allows the fingerprint identification of the compounds. For example, amphetamine, ephedrine, and meperidine can be readily identified. A double-beam recording spectrophotometer is used to blank out the benzene absorption by placing the cyclohexane benzene or heptane-benzene solvent mixture in the reference path.

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