Physico-chemical standardization is a pre-requisite in quality control of unani drugs both single as well as compound formulation as the efficacy of the drugs mainly depends upon their chemical and physical properties. Therefore, the determination of physico-chemical characters for the authenticity of a drug is necessary before studying it for pharmacological activity. In the present study a pharmacopeial compound formulation Laooq Sapistan Khyaar Shambari (LSKS) has been selected to confirm its parameter according to the guidelines given in Unani Pharmacopeia of India (UPI) 2007. The parameters studied for quality assurance of LSKS includes Successive Extractive Value viz. petroleum ether 0.80 ± 0.05, diethyl ether 0.24 ± 0.01, chloroform 0.80 ± 0.05, ethanol 19.78 ± 0.85, aqueous 56.10 ± 0.95, moisture content 3.28 ± 0.02,total ash 0.97 ± 0.00, acid insoluble ash 0.63 ± 0.01,water soluble ash 0.31 ± 0.00 and water soluble matter 42.33 ± 1.20, and alcohol soluble matter 54.33 ± 0.88, specific gravity 1.360±0.011,viscosity at 70% 2310.07, pH Value at 1 % aqueous solution 6.43 ± 0.00 and at 10 % aqueous solution 5.80 ± 0.00, and loss on drying at 105 0C 6.27 ± 0.02. The qualitative analysis of various phytochemicals was estimated that revealed the presence of carbohydrates, glycosides, phenols, proteins, steroids and resins. The TLC profile of this pharmacopoeial formulation was also performed. This study will help in setting down pharmacopoeial standards in determining the quality and purity of compound drug formulation which is in use since time immemorial in URTI and it is also reported to have a potent in-vitro antibacterial activity.