P-Phenylenediamines (PPDs) and its related chemicals have been widely used in the production industry of tires, belts, hoses and cables, and they are considered to be a group of very effective chemical antioxidants, anti-bending cracking agents, and provide excellent ability to protect rubber and its products from thermal degradation and decomposition [1]. Due to the widespread use of rubber products, PPDs has existed in the natural environment for decades, and it is oxidized by ozone to produce PPD-quinone. It has been reported that the half-life of PPD-quinone in water is at least five times that of PPD, and it is strongly toxic to aquatic organisms, with as little as 95ng/L killing young salmon [2]. At present, the commonly used detection methods for p-phenylenediamine and its metabolites are GC-MS and HPLC, which have high detection limits and serious false positive interference. In this study, SCIEX Triple Quad™ system was used to establish four methods for the detection of p-phenylenediamine compounds and 6PPD-quinone, which has the advantages of simplicity, high sensitivity and good accuracy, and provides a valuable means for the public and government regulators to monitor and detect this emerging environmental pollutant.