[a] 1Introduction Nanotechnology is one of the most promising and innovative fields of scientific knowledge [1,2].T aking into account the need to developm ore sensitive and selective electrochemical sensors,t he interest arises from the use of chemically modified electrodes with hybrid nanomaterials,s uch as nanoparticles and carbonaceousm aterials, which may produce synergistic effects,p romoting an improvement in the sensor properties when compared with the sensors by usingasingle material [3,4].Thec arbon black (CB)i sa ni nteresting nanostructured material that has been the target of increasing interesti n electrochemical studies,d ue to its attractivee lectrochemical properties:h igh conductivity,c hemical stability,l arge specific surfacea rea, ability to produce stable dispersion withoutt he need for sophisticated procedures,a nd the fact that it is an extremely cheap material [5][6][7][8][9].F urthermore,t he incorporation of other materials in the CB can improve their properties,i ncreasing the sensitivity and improving the electron transfer between the electroactive speciesa nd the electrode.S everal metal nanoparticles, such as gold [10][11][12][13] Then ickel oxiden anoparticles (NiONPs)a re an important nanomaterial due to the specific chemical, surface and microstructural properties [28].N evertheless,f ew analyticalm ethods using NiONPs-modified electrodes have been described in the literaturef or different analytes [29][30][31][32].B atchelor-McAuley et al. [29] immobilizedN iONPs on ag raphite electrode and applied this for the determination of aspirin. NiONPs-modified GCE also was used to investigate the electrochemical oxidation of amino acids [31]a nd glutathione [32].R ecently,F igueiredoFilho et al. have applied an electrode modified with carbon nanotubes and NiONPs for the simultaneous determination of catecholamine neurotransmitters [30].As far as we could ascertain, NiONPsÀCB-modified electrodes have not been reported. Thus,t his attractive work has encouraged us to investigate the use of glassy carbon electrodes modified with NiONPs and CB for the simultaneous determination of paracetamol( PCT) and codeine (COD).PCT (also knowna sa cetaminophen) is an on-steroidal analgesict hat is widely used for the relief of minor pain and fever [33,34].C OD is an opioid derived from morphine;i ti sc ommonly utilized in combination with other drugs,s uch as aspirin and PCT,b ecause it is difficult to achieve effective moderate to severe pain controlu sing an analgesic alone.T he combination of these drugso ffers effective analgesia at reduced doses of individual agents, which may reduce the severity of the relatedd ose [35][36][37][38].T hus,i ti sn ecessary to develop analytical methods for PCT and COD for the quality control of pharmaceuticals,p hysiological function and diagnosis in clinical mediAbstract:I nt his work, as imple and highlys electivev oltammetric methodw as developed for the simultaneous determination of paracetamol (PCT)a nd codeine (COD) in pharmaceuticals and human body fluid...