A novel dry-spinning method for the preparation of zein fiber without using formaldehyde is presented. The fiber thus obtained had good stability to boiling aqueous acetic acid solution with breaking tenacity and elongation of 1.0 g/d and 30%, respectively. Citric acid and butanetetracarboxylic acid were used as nonformaldehyde crosslinking agents for the preparation of zein fiber successfully. Using polycarboxylic acids have advantages such as no toxicity and low sensitivity to the variation of processing conditions over formaldehyde-containing stabilizers. The effects of crosslinking before and after stretching on improvement of fiber properties were discussed. Fiber morphological structure was also examined by means of wide angle x-ray diffraction and sonic velocity.