The physiological environment is a crucial factor in biomedical systems, which can be regulated with relative ease both in vitro and in vivo.

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Phosphorylated κ‐carrageenan has the potential to exhibit higher antioxidant activity than other polysaccharides. Low‐molecular‐weight κ‐carrageenan polysaccharides (LMW κ‐CAR) were prepared through oxidative degradation of high‐molecular‐weight κ‐carrageenan, and LMW κ‐CAR subjected into phosphorylation. Phosphorylated κ‐carrageenan (PCAR)‐chitosan (CS) nanoparticles was prepared by emulsification technique, followed by ionic gelation technique. Rifampicin (RF) and isoniazid (INH) were used as model drugs and encapsulated in CS‐PCAR nanocarriers. The encapsulation of drugs (RF and INH) in the CS‐PCAR polymeric carrier was verified by Fourier transform infrared spectroscopy (FT‐IR). The analysis of X‐ray diffraction (XRD) data demonstrated both RF and INH were loaded in the CS‐PCAR nanocarrier in an amorphous form. As observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), CS‐PCAR nanoparticles shows spherical structure with soft surface and exhibited good aggregation, whereas INH and RF loaded CS‐PCAR nanoparticles had varying shapes like hexagonal, that indicates their different compositions and structures. Encapsulation efficiency was determined by UV‐Vis, which was interrelated to the initial concentration of INH and RF. Cumulative release of RF and INH from CS‐PCAR nanoparticles was observed in in‐vitro studies. An initial, tremendous release was observed from both RF and INH drug formulated carriers, which was followed a regular prolonged releases. The outcome of the drug release was controlled by their drug quantity, indicating that the discharge could be suffered by concentration of drug. The results suggest that CS‐PCAR nanoparticles are a pretty system for simultaneous release of RF and INH in the treatment of tuberculosis.