In the present study, an efficient and inexpensive Air-assisted liquid-liquid microextraction (AALLME) technique was used to extraction and determination of chlordiazepoxide in tablet formulation by HPLC-UV. Chlordiazepoxide (7-chloro-N-methyl- 5-phenyl-3H-1,4-benzodiazepine-2-amino-4-oxide) is one of benzodiazepines category that has medicine properties such as antianxiety, sedative, anticonvulsant, and muscle relaxant. This compound has high half-life time (between 40 and 140 h) [1]. Therefore, it has great effect on the actions of other benzodiazepines and used for the treatment of anxiety disorders or short-term relief of anxiety symptoms, relieve anxiety, and tension, and control of agitation associated with acute alcohol withdrawal. [2–4]. The effects of various parameters such as pH of the sample solution, salt addition, the volume of extraction solvent, and the number of extraction cycles were investigated. The optimized extraction condition were extraction solvent volume = 300 μl, number of extraction = 12 cycle, salt concentration = 10% w/v, without pH adjusment. Satisfactory results were obtained with enrichment factor and recovery equal to 116.31 and 81.42% respectively. The method has been successfully applied for the analysis of chlordiazepoxide in tablet formulation.