Abstract: Headspace-Solid Phase Microextraction (HS-SPME) in combination with Gas Chromatography-Mass Spectrometry (GC-MS) is currently used for identification of Volatile Organic Compounds (VOCs) in food and environmental samples. Although, HS-SPME is a reliable technique with good sensitivity and selectivity, several factors must be thoroughly considered for accurate and precise quantification of VOCs. This study focuses on the state of the art review for quantitative determination of VOCs using the same in both air and water samples. Selections of appropriate techniques for generating external calibration in conjunction with the experimental findings on meat VOCs are also presented. A simple laboratory set up was designed for generation of calibration curves for ethanol and acetic acid and statistically significant reproducibility were obtained for the same.