A new data processing method for in vivo NMR data quantitation is presented. This method (EPLPSVD) is based on the enhancement procedure (EP) proposed by J. A. Cadzow (IEEE Trans. Acoust. Speech Signal Process. 36, 49, 1988) followed by the usual linear prediction method using the singular value decomposition (LPSVD). The evaluation of this protocol is performed using synthesized 31P signals with different signal-to-noise ratios. A Monte-Carlo simulation as a function of signal-to-noise ratio (SNR) has proved that EPLPSVD leads to unbiased estimated values of parameters. Then the Cramer-Rao method yields reliable confidence intervals for the estimated parameters. The estimates of NMR parameters using EPLPSVD are reliable and accurate for SNR > or = 1.2 while the LPSVD method failed for SNR < or = 4. This protocol is applied to analyze automatically a series of 31P free induction decays obtained from the human gastrocnemius muscle during exercise. Spectral parameters with their confidence intervals, curves of relative intensity variations in phosphocreatine and inorganic phosphate, and pH curves are automatically provided.