Improvement and validation the method using dispersive liquid–liquid microextraction with in situ derivatization followed by gas chromatography–mass spectrometry for determination of tricyclic antidepressants in human urine samples

A simple, rapid and sensitive method termed dispersive liquid–liquid microextraction (DLLME) combined with gas chromatography–mass spectrometry (GC/MS) was developed for the determination of tricyclic antidepressants (TCAs) in human urine sample. An appropriate mixture of methanol (disperser solvent), carbon tetrachloride (extraction solvent), and acetic anhydride (derivatization reagent) was injected rapidly into human urine sample. After extraction, the sedimented phase was analyzed by GC/MS. The calibration curves obtained with human urine were linear with a correlation coefficient of over 0.99 in the range of 2.0/5.0–100 ng mL−1. Under the optimum conditions (carbon tetrachloride: 10 μL, methanol: 150 μL), the detection limits and the quantification limits of the tricyclic antidepressants were 0.5–2.0 ng mL−1 and 2.0–5.0 ng mL−1, respectively. The average recoveries of TCAs were 88.2–104.3%. Moreover, the inter- and intra-day precision and accuracy was acceptable at all concentrations. The results showed that DLLME is applicable to the determination of trace amounts of TCAs in human urine sample.

► In situ derivatization-DLLME-GC/MS method was validated and developed.
► TCAs in human urine sample were determined by that suitable method.
► Proposed method has many practical advantages, and was achieved high sensitivity.