Fast magic-angle spinning (≥60 ​kHz) technique has enabled the acquisition of high-resolution ¹H NMR spectra of solid materials. However, the spectral interpretation is still difficult because the ¹H peaks are overlapped due to the narrow chemical shift range and broad linewidths. An additional ¹³C or ¹⁴N or ¹H dimension possibly addresses the issues of overlapped proton resonances, but it leads to the elongated experimental time. Herein, we introduce a single-channel ¹H experiment to separate the overlapped ¹H peak and identify its spatially proximal ¹H–¹H correlations. This sequence combines selective excitation, selective ¹H–¹H polarization transfer by selective recoupling of protons (SERP), and broadband ¹H recoupling by back-to-back (BABA) recoupling sequences. The concept for ¹H separation is based on (i) the selective excitation of a well-resolved ¹H peak and (ii) the selective dipolar polarization transfer from this isolated ¹H peak to one of the ¹H peaks in the overlapped/poor resolution region by SERP and (iii) the detection of ¹H–¹H correlations from these two ¹H peaks to other neighboring ¹Hs by BABA. We demonstrated the applicability of this approach to identify overlapped peaks on two molecules, β-L-aspartyl-l-alanine and Pioglitazone.HCl. The sequence allows the clear observation of ¹H–¹H correlations from an overlapped ¹H peak without an additional heteronuclear dimension and ensures efficient polarization transfers that leads to twelve fold reduction in experimental time compared to ¹⁴N edited experiments. The limitation and the conditions of applicability for this approach are discussed in detail.

快速魔角旋转（≥60 kHz）技术能够获取固体材料的高分辨率¹ H NMR 光谱。然而，光谱解释仍然很困难，因为¹ H 峰由于窄化学位移范围和宽线宽而重叠。额外的¹³ C 或¹⁴ N 或¹ H 维度可能解决重叠质子共振的问题，但会导致实验时间延长。在这里，我们介绍了一个单通道¹ H 实验来分离重叠的¹ H 峰并识别其空间上接近的¹ H - ¹H 相关性。该序列结合了选择性激发、通过质子选择性再耦合 (SERP) 进行的选择性¹ H – ¹ H 偏振转移和通过背靠背 (BABA) 再耦合序列进行的宽带^{1 H 再耦合。1} H 分离的概念基于 (i) 良好分辨的¹ H 峰的选择性激发和 (ii) 从这个孤立的¹ H 峰到重叠/差的¹ H 峰之一的选择性偶极极化转移SERP 的分辨率区域和 (iii)从这两个¹ H 峰到其他相邻^1的1 H - ^{1 H 相关性的检测}来自 BABA 的 Hs。我们证明了这种方法在识别两个分子 β-L-天冬氨酰-1-丙氨酸和吡格列酮.HCl 上的重叠峰的适用性。该序列允许从重叠的^{1 H 峰清楚地观察1} H - ^{1 H 相关性，而无需额外的异核尺寸，并确保有效的极化转移，与14} N 编辑实验相比，导致实验时间减少 12 倍。详细讨论了这种方法的局限性和适用条件。