In the present work, we direct carbonization ZIF-67, by used zeolitic imidazolate framework (ZIF-67) as precursor to prepare porous carbon-ZIF-67. By applying a post-carbonization acidic etching treatment with hydrofluoric acid (HF), the initial surface area of the carbon-ZIF-67 sample increased. For applied applications, the porous carbon-ZIF-67-HF material was used to fabricate a carbon composite membrane using polyvinylidene difluoride (PVDF) membrane. The prepared membranes were applied as sorbent for thin film microextraction (TFME) of diclofenac sodium in biological fluids. After elution, diclofenac sodium was quantified by high performance liquid chromatography-ultraviolet detection (HPLC-UV).