Burrow Timothy E, Burns Darcy C, Krishnamurthy Krish, Reynolds William F
Department of Chemistry, University of Toronto, Toronto, Ontario, Canada.
Magn Reson Chem. 2014 May;52(5):195-201. doi: 10.1002/mrc.4050. Epub 2014 Feb 19.
A modified version of the attached proton test (APT) sequence for (13)C spectral editing, which we call CRisis-APT (CRAPT), is developed and tested on representative organic compounds. CRAPT incorporates (13)C compensation for refocusing inefficiency with synchronized inversion sweeps (CRISIS) pulses in combination with (1)H broadband inversion pulses to give improved compensation for variations in (1)JCH along with improved refocusing efficiency. It is shown that CRAPT gives edited (13)C spectra with only small losses in sensitivity (between 8% and 15% for strychnine, 1, menthol, 2, cholecalciferol, 3, and isotachysterol, 4), compared with basic (13)C spectra obtained on the same compounds. CRAPT also gives significantly better signal/noise than DEPTQ for nonprotonated carbons. Therefore, we conclude that CRAPT is an improvement over APT or DEPTQ or a combination of DEPT135 with a full (13)C spectrum for routine (13)C spectral editing of organic compounds.
我们开发了一种用于(13)C谱编辑的附加质子测试(APT)序列的修改版本,称为CRisis-APT(CRAPT),并在代表性有机化合物上进行了测试。CRAPT结合了(13)C补偿,以补偿同步反转扫描(CRISIS)脉冲的重聚焦效率低下问题,并结合(1)H宽带反转脉冲,以更好地补偿(1)JCH的变化以及提高重聚焦效率。结果表明,与在相同化合物上获得的基本(13)C谱相比,CRAPT给出的编辑后的(13)C谱灵敏度损失很小(士的宁为8%至15%,薄荷醇为1,胆钙化醇为2,异速甾醇为3和4)。对于非质子化碳,CRAPT的信号/噪声也明显优于DEPTQ。因此,我们得出结论,对于有机化合物的常规(13)C谱编辑,CRAPT是对APT或DEPTQ或DEPT135与完整(13)C谱组合的改进。