A simple, rapid, and environmentally-friendly spectrophotometric method for nitrite detection was developed. Detection was based on a redox reaction with iodide ions in an acidic condition. The reaction was evaluated by detecting the increase in absorbance of the colored product of iodine at 362 nm wavelength. To obtain a good spectrophotometric performance, the iodide ions concentration, hydrochloric acid concentration, and reaction time were optimized. In the optimal condition, the developed spectrophotometric method provided a linear range of 0.0625 to 4.00 mg L−1 (r = 0.9985), reaction time for 10 min, a limit of detection of 25 µg L−1, and a limit of quantitation of 85 µg L−1. This method showed good repeatability (RSD −1), and good accuracy (recovery = 88 ± 2 to 99.5 ± 0.4%). The method has the potential to be used in crime scene investigations as a rapid screening test for gunshot residue detection via nitrite detection.