The aim of this research was to identify the effects of NPS fertilizer with the spraying of Nano-NPK+TE and Cerium Oxide NPs on the active substances in rice grains, amber 33 cultivar. This field study was carried out in the Tali’a region, 41-Husainiya, Hilla city, Babylon province, Iraq, from 14/6/2022 to 25/11/2022, The study treatments were randomly distributed on the experimental units according to a simple and one-way experiment by a randomized complete block design (RCBD). The study treatments consisted of adding NPS fertilizer at four levels (0, 100, 200, and 300 kg ha-1) and spraying with nanomaterials of Nano-NPK+TE and Cerium Oxide NPs at concentrations of (2.5 ml L-1) and (50 mg L-1), respectively, with four sprays for each of them. A total of 16 experimental units were used. The Statistical analysis using the least significant difference test revealed that the process of fertilizing with NPS fertilizer and nanomaterials led to significant differences and an increase in the contents of volatile oils, saturated and unsaturated fatty acids among the dietary components of rice grains, so the findings from gas chromatography-mass spectrometry (GC-MS) analysis indicated that soil fertilization with NPS mineral fertilizer at level (300 kg ha-1) achieved the highest level of stearic acid content with a value of (9.460%), as well as the highest improvement in Palmitic acid content (24.240%) recorded by the treatment (NPS 100 kg ha-1). Moreover, the bi-combination of NPS (200 kg ha-1) + Spray CeO2 NPs gave the highest content of Oleic acid content in percentage (10.310%), and Linoleic, another type of unsaturated fatty acid, indicated a content of (10.020%) by the combination of (NPS (300 kg ha-1) + Spray nano-NPK+TE). Additionally, the highest percentage of Volatile oils showed at the foliar spraying combination (Spray nano-NPK+TE + CeO2 NPs), which gave a value of (46.50%).