Diazepam is an important member of the group of 1,4-benzodiazepine derivatives, which have found extensive use in current therapy. It is used for the symptomatic relief of tension and anxiety, acute alcohol withdrawal, adjunct therapy in skeletal muscle apasms and is preferred by many clinicians for the management of status epilepticus. 1 Nowadays, diazepam is the drug of choice for the control of acute seizures. It is inexpensive, widely available in resourcepoor countries and effective when given by the intravenous or rectal routes. When such drugs are used singly, they appear to be relatively safe, but are of significant pharmacological importance when in the presence of other depressant drugs, such as barbiturates, narcotics and phenothinzines. 2 The wide use of these drugs necessitates a rapid, reliable and sensitive method for their quantitation.Numerous analytical techniques based on gas chromatography, 3 high performance liquid chromatography, 4,5 capillary electrophoresis, 6 TLC-densitometry, polarography, 7 the electrochemical method 8 and spectrophotometry 9 have been developed for determining benzodiazepines in various sample matrices. For examples, Yu et al. 10 described a second-order derivative spectrometric method for diazepam determination in commercial injection. Measurements were made at 343, 339, 335, 323, 319 and 315 nm. The mean recovery (n = 3) of diazepam was 100.3% with a coefficient of variation of 0.6%.A reversed-phase HPLC procedure with UV detection was reported for diazepam determination in plasma samples from children with severe malaria. 11 Liu et al. 12 described an RP-HPLC method for the quantitation of diazepam and its metabolites in dog plasma. A flow injection (FI) fluorometric determination of diazepam and other benzodiazepines in pharmaceutical preparations after hydrolysis was developed. 13 Recently, a derivative UV spectrophotometric method has been proposed for the simultaneous determination of phenylpropanolamine hydrochloride, caffeine and diazepam in tablets. Satisfactory results were obtained and were in good agreement with those obtained by RP-HPLC. 14 A thin-layer chromatographydensitometry technique has been developed for the separation and determination of diazepam and other benzodiazepine derivatives in tablets. 15 TLC-densitometry, although the yield has slightly higher values than the HPLC method, is preferred, owing to its simplicity, ease and low-cost. Salem et al. 16 described spectrophotometric and fluorometric methods for determining diazepam, bromazepam and clonazepam in pharmaceutical and urine samples. The methods are based on measuring the absorption or emission spectra in a methanolic potassium hydroxide solution. Fluorometric methods have proved to be selective with low detection limits (7.13 ng mL -1 ), whereas spectrophotometric methods show relatively high detection limits (1.27 µg ml -1 for diazepam). However, many of such procedures have been criticized as being tedious, time consuming with occasionally suffer from lack of selectivity. Some mod...