Microwave-assisted hydrolysis and extraction of tricyclic antidepressants from human hair

The objective of this research was to develop, optimize, and validate a modern, rapid method of preparation of human hair samples, using microwave irradiation, for analysis of eight tricyclic antidepressants (TCADs): nordoxepin, nortriptyline, imipramine, amitriptyline, doxepin, desipramine, clomipramine, and norclomipramine. It was based on simultaneous alkaline hair microwave-assisted hydrolysis and microwave-assisted extraction (MAH–MAE). Extracts were analyzed by high-performance liquid chromatography with diode-array detection (HPLC–DAD). A mixture of n-hexane and isoamyl alcohol (99:1, v/v) was used as extraction solvent and the process was performed at 60°C. Application of 1.0 mol L−1 NaOH and microwave irradiation for 40 min were found to be optimum for hair samples. Limits of detection ranged from 0.3 to 1.2 μg g−1 and LOQ from 0.9 to 4.0 μg g−1 for the different drugs. This enabled us to quantify them in hair samples within average therapeutic concentration ranges

ANALYSIS OF ILLICIT DRUGS IN HUMAN BIOLOGICAL SAMPLES BY LC-MSn

There are several classes of illegal substances with different psychotropic effects. It is possible to select a biological matrix and a suitable analytical strategy depending on the aim of the analysis and/or on the availability of the sample or on which kind of information is needed. Liquid chromatography–mass spectrometry (LC-MS or LC-MS/MS) has provided a helpful tool in this field especially for hydrophilic, thermolabile, and nonvolatile analytes, which analysis is sometimes critical by gas chromatography–mass spectrometry (GC-MS). Specific guidelines or procedures have been adopted in order to assist the chemist and to direct him/her towards the practical applications, for which a new analytical method is being created, including measures of verification and external assessment. [...