The evolution and functioning of various tropical ecosystems is poorly understood due to a lack of quantitative techniques to characterize the physicochemical composition of soils and sediment. Here, a detailed multi-method study of lithological changes is provided from a core taken from the silted-up Dibi subsidence lake (central Cameroon). To unravel the provenance of sediment, mineral constituents, and organic matter sources, an array of tools are applied including a spectrophotometer, a laser particle sizer, Rock-Eval pyrolysis, X-ray diffractometer (XRD), a portable X-ray fluorescence (XRF) spectrometry, and an inductively coupled plasma-atomic emission spectroscopy (ICP-AES) instruments. The studied core consists of light-colored deposits at the base (Unit 1) overlain by dark humic deposits (Unit 2). The sediment is very well graded (grading index Sd < 0.35Ф), indicative of bottom suspended to rolling transport. Unit 1 is characterized by relatively low values of total organic carbon (TOC: 2%–5%) whereas the dark Unit 2 has high contents of TOC (10%–33%). The core shows a high oxygen index (OI) value (average = 207 mg carbon dioxide (CO2)/g TOC) and a low hydrogen index (HI) value (average = 107 mg hydrocarbon (HC)/g TOC). This indicates highly altered organic matter (OM), likely from decomposed terrestrial plants. The chlorophyll-α fingerprint (peak around 675 nm) also reveals an autochtonous primary production of organic matter. The mineralogical assemblage of Unit 2 comprises kaolinite, quartz, feldspars, montmorillonite, ilmenite, siderite, gibbsite, rutile, and anatase whereas that of Unit 1 is similar but differs with the presence of illite and the absence of gibbsite. The high titanium dioxide (TiO2) and zirconium (Zr) contents confirm that the source rocks also are comprised of granites, and gneiss without volcanic rocks, such as basalts and trachytes. The source rocks have been intensively weathered using some parameters such as ln(Al2O3/Na2O), K2O/Rb, K/Al, and weathering indices, where Al2O3 denotes aluminum oxide, Na2O denotes sodium oxide, K2O denotes potassium oxide, Rb denotes rubidium, K denotes potassium, and Al denotes aluminum. The enrichment factors (EF) of redox-sensitive trace elements and their relation with TOC, the negative values of manganese/iron ratio (Mn∗) associated to three elemental ratios (cupper/zinc (Cu/Zn), thorium/uranium (Th/U), and vanadium/chromium (V/Cr)) attest to the predominance of sub-oxic to anoxic bottom waters in Dibi lake during sediment deposition. The data also show low primary productivity at the base of the core, followed by an increase towards the top, linked to the intensification of weathering and facilitated by humid climatic conditions, usually increase terrestrial input and palaeoproductivity. The petrological data show a generally warm and humid palaeoclimate. This climatic variation has contributed to the large spread of the savannah and disappearance of the forest. This study sheds light on the late Pleistocene to Holocene palaeoenvironment evolution of the Adamawa region which could be integrated into the context of the Pleistocene to Present regional evolution of the tropical palaeoenvironment.