Highly efficient preconcentration of anti-depressant drugs in biological matrices by conducting supramolecular solvent-based microextraction after dispersive micro solid phase extraction technique

• Two methods were used in a raw for preconcentration of anti-depressants before HPLC analysis . • Dμ-SPE coupled SSME was exploited for determination of ultra-trace levels of these drugs. • The devised method was selective, sensitive, green, and highly beneficial. • Wide linearities, acceptable RSD values, and good LODs and LOQs were obtained. • The devised method was tested for analysis of biological samples with complex matrices. A selective, sensitive, and green sample preparation method was devised by applying a supramolecular solvent-based microextraction (SSME), based on the salting out effect, after conducting the dispersive micro solid phase extraction (Dμ-SPE). The technique was employed for preconcentrative extraction and determination of five anti-depressant drugs in human plasmas and urine samples. The first step was conducted by synthesizing and using a layered double hydroxide-carbon nanotube nanohybrid adsorbent. Multiple interactions betwixt the nanoadsorbent and target analytes, including electrostatic, hydrogen bonding, and π-π interactions and the large surface area of the adsorbent led to an effective performance. In the next step, after emulsification in the presence of supramolecular solvent by ultrasonication, the salting-out effect was applied to separate the extraction phases. At Optimization conditions, wide linearities were obtained, in the ranges of 1.5–3500, 2.0–3500, 1.0–3200, 2.0–3000, and 2.0–3000 ng mL −1 for imipramine, amitriptyline, trimipramine, sertraline, and citalopram, respectively, with low limits of detection ranging from 0.3 to 0.6 ng mL −1 . Also, acceptable RSD values (≤8.9%; n = 5) for intra- and inter–day precision were obtained, along with acceptable spiked recoveries (94.5–100.0%) in complex matrices. Overall, the effectiveness of the nanosorbent, ultrasonication, supermolecule green solvents with easy solidification and collection, and elimination of the centrifugation bestowed a highly beneficial method for analyzing anti-depressant drugs.