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Determination of Diltiazem in Post-Mortem Blood by High-Performance Liquid Chromatography

NCJ Number
Problems of Forensic Sciences Volume: 53 Dated: 2003 Pages: 22-37
Marianna Kiska; Roman Madro
Date Published
16 pages
This article presents the analytical conditions used in the determination of diltiazem (D) and deacetyldiltiazem (DAD) in postmortem blood using high-performance liquid chromatography (HPLC) a simple method of preparing DAD is described.
Extraction and analysis by the HPLC method enabled the determination of both D and DAD in postmortem blood at concentrations similar to the upper limit of therapeutic levels, i.e., from 0.5 mg/ml. In the diagnosis of fatal poisonings with D in blood received from a corpse, the level of DAD should also be determined; it is not only one of the main metabolites of D, but also a product of decomposition of this xenobiotic in blood in vitro. The conditions of controlled hydrolysis of D in the acidic environment presented in this paper make it possible to obtain DAD, which is suitable as a standard for quantitative analysis. Due to its wide use in treating angina pectoris, arterial hypertension, and arrhythmia, D is sometimes the cause of acute intoxication or death. D and DAD were isolated from blood by liquid-liquid extraction in a moderately alkaline medium with application of a mixture of dichloromethane and ether and determined with a liquid chromatograph, using Hypersil ODS (250 x 4mm, 5mm) column; a mobile phase of 1.5 ml/min flow in an isocratic system of two pumps, consisting of acetonitrile and phosphate buffer at pH = 3 (0.025 M solution of phosphoric acid with the addition of 6 ml of triethylamine per 1 liter) in proportions 25:75; and ultraviolet detection at 235 nm. 1 table, 6 figures, and 24 references


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