Proton decoupled 31P in vivo NMR spectroscopy of the human finger flexor muscles was performed during exercise and recovery using a 1.5 T whole-body imager. Predominantly the gamma-ATP signal shows a splitting caused by different signal contributions with chemical shifts that vary independently. Studies on the human gastrocnemius and biceps femoris muscle were undertaken to investigate the appearance of the splitting in these muscles as well. In all cases more than one signal contribution was found which might represent the different muscle fibre types and their recruitment pattern following exercise. An analysis of the chemical shifts (delta) of ATP results in changes of up to 0.4 ppm and 0.1 ppm for delta gamma- and delta beta-ATP, respectively. Based solely on the chemical shifts of the ATP 31P signals the tissue pH value following exercise was determined. The result was in good agreement with the value derived from delta Pi.
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