Pharmaceuticals and personal care products (PPCPs) are becoming a growing concern in aquatic environments due to their impact on human health and the environment. Chloramphenicol (CAP) [1] is a commonly used antibiotic that is difficult to remove from water sources and can lead to drug-resistant bacteria. Advanced Oxidation Processes (AOPs) [2] and sonochemistry are effective methods for removing pollutants from water, and Layered Double Hydroxide (LDH) has excellent adsorption properties for heavy metal ions. Layered metal-free graphitic carbon nitride g-C3N4 [3] has potential as a sonocatalyst for degrading pollutants, but its efficiency can be improved by loading heteroatoms or creating heterojunctions with other semiconductors. The NiFe LDH/g-C3N4 double layered hydroxide nanocomposite shows promise for efficient sonocatalytic degradation of pharmaceutical pollutants.