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Manual headspace-solid phase microextraction (HS-SPME) in combination with gas chromatography-mass spectrometry (GC-MS) is one of the preferred methods, currently used for the identification of volatile organic compounds (VOCs) in food and environmental samples. HS-SPME is an inexpensive, solvent-free and reliable technique with excellent sensitivity and good selectivity. Though it is an excellent technique for identification of VOCs in food and environmental samples, several factors that affect SPME must be thoroughly considered for accurate and precise quantification. The paper focuses on the state-of-the-art review for quantitative determination of organic compounds using the same in both air and water samples. Selection of appropriate techniques for generating external calibration in conjunction with our ongoing study and the associated findings are also presented.