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It was introduced by Harmon Northrop Morse in R428 order 1877. It is classified as a mild pain reliever that is commonly used for the relief of headaches and other minor aches and pains. It is approved for reducing fever in people of all ages. Also, it is used for the relief of pains associated with many parts of the body that is comparable to that of aspirin, while its anti-inflammatory effects are weaker. It is better tolerated than aspirin in patients in whom excessive gastric acid secretion or prolongation of bleeding time may be a concern. Untreated acetaminophen overdose results in a lengthy and painful illness. Signs and symptoms of acetaminophen toxicity may initially be absent or nonspecific symptoms. The process of dying from an overdose usually takes three to five days [20, 21]. In the last decade, numerous methods have been reported for the analysis of acetaminophen in pharmaceutical samples and biofluids. They are including colorimetry [22], spectrophotometry [23], NIR spectroscopy [24], capillary electrophoresis [25], microemulsion liquid chromatography [26], high performance liquid chromatography [27, 28], and electrochemical methods that are the most conventional methods [29�C34]. Acetaminophen in combination with opioid analgesics like codeine can also be used in the management of more severe pain such as postsurgical pain and providing palliative care in advanced cancer patients and improving the efficacy for about 50% of patients [35]. Therefore, quantitative determination of codeine and acetaminophen individually or in the presence of both is important from E-64 different points of view. To the best of our knowledge, up to now, there was not found any report for the simultaneous determination of codeine and buy JQ1 acetaminophen using electrochemical methods. In continuing of our research on the fabrication of 4-hydroxy-2-(triphenylphosphonio)phenolate (HTP)/multiwall carbon nanotubes modified carbon paste electrode (HTP-MWCNT-CPE) and its applications for the determination of different analytes [19, 36], we introduced a sensitive and selective sensor for the individual and simultaneous determination of codeine and acetaminophen using HTP-MWCNT-CPE for the electrocatalytic oxidation of codeine and the simultaneous determination of codeine and acetaminophen. The modified electrode shows excellent electrocatalytic activity toward codeine with low detection limit and wide linear dynamic range. Moreover, the modified electrode exhibits good ability for simultaneous determination of codeine and acetaminophen in serum and urine samples as biological and acetaminophen and acetaminophen-codeine tablet as pharmaceutical samples. 2. Experimental 2.1. Apparatus and Chemicals All the electrochemical measurements were carried out using an Autolab potentiostat-galvanostat PGSTAT 30 (Eco Chemie, Netherlands) equipped with GPES 4.9 software.