In this work, a molybdenum-based coordination polymer {[Mo(PDA)(NO)(μ-O)MoO3]·1.42H2O·0.58C2H5OH}n (1) (PDA is 1,10-phenanthroline-2,9-dicarboxylate) was synthesized using solvothermal reaction conditions and characterized using a suite of analytical techniques. The utility of 1 as a sorbent for the dispersive micro solid-phase extraction (D-μSPE) of basic organic compounds such as antidepressants is supported by the thermal stability of the coordination polymer (up to ∼400 °C). The crystalline material also shows excellent hydrolytic stability with negligible decomposition observed in water over seven days. Besides, the material shows a modest resistance to decomposition for around 24 hours upon exposure to strongly acidic pH 2.0 or strongly basic media pH 10.0. Single-crystal X-ray diffraction studies reveal a 1D chain structure, with close contacts expanding the structure into three dimensions including π-interactions and hydrogen bonding. Therefore, due to the thermal/moisture/chemical stability of 1 as well as the presence of extensive electrostatic interactions and functional groups in it, 1 can be a suitable choice as sorbent in the D-μSPE of antidepressant drugs from human plasma samples via appreciable adsorbate-adsorbent interactions. Analysis of the extracted antidepressant drugs was conducted using high- performance liquid chromatography-ultraviolet (HPLC-UV), with calibration plots being linear in the concentration range of 0.1−500 ng mL‒1 for amitriptyline and nortriptyline, 0.2‒ 500 ng mL‒1 for imipramine, and 0.5‒300 ng mL‒1 38 for sertraline. The relative standard deviation (RSD) values were calculated for both intra-day and inter-day precision and the RSD% values were in the range of 3.9 to 5.2% and 4.6-5.4%, respectively. The limits of detection (LODs) was determined as 0.03-0.2 ng mL‒1 , with the D-μSPE-HPLC-UV method proving valid for the analysis of antidepressant drugs in human plasma samples with recoveries of the analytes in the range of 94.9 to 102%.

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