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In order to improve the efficiency of Soxhlet extraction and oven drying, low-field nuclear magnetic resonance (LF-NMR) technology was used to detect fat and moisture contents in pork. The transverse relaxation time (T2) distribution curves were constructed by Carr–Purcell–Meiboom–Gill (CPMG) experiments. In addition, the optimal conditions of adding MnCl2 aqueous solution was explored to separate water and fat signal peaks. Finally, the reliability of this method for the determination of fat and moisture contents in pork was verified. The present study showed that adding 1.5 mL of 20% MnCl2 aqueous solution solution at 50 °C can isolate and obtain a stable peak of fat. The lard and 0.85% MnCl2 aqueous solution were used as the standards for fat and moisture measurements, respectively, and calibration curves with R2 = 0.9999 were obtained. In addition, the repeatability and reproducibility of this method were 1.71~3.10%. There was a significant correlation (p < 0.05) between the LF-NMR method and the conventional methods (Soxhlet extraction and oven drying), and the R2 was 0.9987 and 0.9207 for fat and moisture, respectively. All the results proved that LF-NMR could determine fat and moisture contents in pork rapidly and simultaneously. [ABSTRACT FROM AUTHOR]