<p>Termites are a natural component of the diet of Malayan pangolins, whereas artificial diets used under captive conditions may differ substantially from wild prey in structure and composition, particularly in chitin content. This study evaluated the effects of dietary supplementation with termites or chitin in seven captive male Malayan pangolins exposed sequentially to three dietary conditions: artificial diet alone, artificial diet supplemented with termites, and artificial diet supplemented with chitin. Body weight, hematological and serum biochemical parameters, fecal scores, and gut microbiota composition were assessed. The results showed that the effects of termite and chitin supplementation were not consistent. Compared with the other dietary phases, chitin supplementation was associated with body weight reduction in some individuals and changes in several physiological parameters, including white blood cells, lymphocytes, mean corpuscular volume, eosinophils, and even significantly reduced in phosphorus, calcium, albumin, and cholesterol (<i>p</i> &lt; 0.05). In the gut microbiota analysis, termite supplementation significantly increased Chao1 richness and observed OTUs (<i>p &lt;</i> 0.05), while the overall microbiota composition differed between the termite- and chitin-supplemented phases. In addition, the chitin-supplemented phase showed a higher relative abundance of some taxa previously reported to be associated with potential pathogenicity. In conclusion, supplementation with termites and chitin produced different physiological and microbiota responses in captive Malayan pangolins. Under the conditions of this study, supplementation with 3% chitin was associated with less favorable outcomes than termite supplementation. Future studies should further evaluate dietary composition, including chitin and other nutrient components, to support the development of optimized diets for captive pangolins.</p>