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Abstract High Resolution–Magic Angle Spinning (HR‐MAS) spectroscopy provides rich biochemical profiles that require accurate quantification to permit biomarker identification and to understand the underlying pathological mechanisms. Meanwhile, quantification of HR‐MAS data from prostate tissue samples is challenging due to significant overlap between the resonant peaks, the presence of short T_2^* metabolites such as citrate or polyamines (T2 from 25 to 100 msec) and macromolecules, and variations in chemical shifts and T_2^* s within a metabolite's spin systems. Since existing methods do not address these challenges completely, a new quantification method was developed and optimized for HR‐MAS data acquired with an ultra short TE and over 30,000 data points. The proposed method, named HR‐QUEST (High Resolution–QUEST), iteratively employs the QUEST time‐domain semi‐parametric …