Discrimination of different types of sulfur-containing species not only helps us to deeply understand how sulfur affects cellular signaling, but also contribute to the early diagnosis of diseases. However, the current investigation about sulfur-containing species discrimination is mainly concentrated in biothiols, which is relatively limited for practical application. Toward circumventing this limitation, herein, a convenient sensor array consisting of three kinds of Au NCs-Cu2+ for simultaneous and rapid identification of different types of sulfur-containing species is reported. Based on the fingerprint-like fluorescence responses generated by competitive binding between Au NCs-Cu2+ and different sulfur-containing species, not only ten different types of sulfur-containing species separately but also their binary or ternary randomly selected mixtures can be well discriminated even in human urine and serum samples. It is worth noting that it only takes 2 min to obtain the best response signals for sulfur-containing species discrimination. Most importantly, serums from cancer patients (such as liver cancer and breast cancer) and healthy people as well as sulfur-oxidizing bacteria (SOB) and sulfur-free bacteria can be both effectively and rapidly identified within 2 min, respectively, making it a promising approach for point-of-care disease diagnostic.