OBJECTIVE To establish a fluorescence spectrophotometry method for the determination of norfloxacin in both capsule and human urine samples.METHODS Study the fluorescent properties of norfloxacin in different pH environment,thus determine the best test condition and quantify norfloxacin in both capsule and human urine samples.RESULTS For capsule sample,the λex and λem was 252 nm and 378 nm,the linear range was 0.01μg·mL-1~1.0μg·mL-1;while for human urine sample,the λex and λem was 290 nm and 448nm respectively,linear range was 0.01μg·mL-1~2.0μg·mL-1。For both samples its detection limit was 0.01μg·mL-1.CONCLUSION This method is easy,swift,sensitive and without interference.It can be applied to the determination of norfloxacin in both capsule and human urine.