Complete 13C resonance assignments of tryptophan in L-lysyl-L-tryptophyl-L-lysine by single-bond and multiple-bond correlated 1H-13C two-dimensional NMR.
Complete 13C resonance assignments of tryptophan in L-lysyl-L-tryptophyl-L-lysine by single-bond and multiple-bond correlated 1H-13C two-dimensional NMR.
复制标题
通过单键和多键相关 1H-13C 二维 NMR 完成 L-赖氨酰-L-色氨酸-L-赖氨酸中色氨酸的 13C 共振归属。
DOI：
10.1002/bip.360281015
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发表时间：
1989
期刊：
影响因子：
2.9
通讯作者：
Markley,JL
中科院分区：
文献类型：
--
作者：
Oh,BH;Markley,JL
材料和方法-赖氨酰-L-色氨酸-L-赖氨酸和L-色氨酸购自Sigma Chemical Co.，并且无需进一步纯化即可使用。用于 nmr 光谱的三肽样品是 50 mM L-赖氨酰-L-色氨酸-L-赖氨酸，溶解在 2.8 mL'H2O 中，含有 100 mM 磷酸盐缓冲液，pH* 7.24（pH 读数未针对氘同位素效应进行校正）。游离氨基酸样品是溶解在二甲基亚砜 (DMSO-d) 中的 28 mM L-色氨酸。所有 nmr 数据均在 25°C 下在 Bruker AM-400 WB nmr 光谱仪上收集，操作频率为 400.13 MHz 的 H 频率和 100.6 MHz 的 I3C 频率。 'H {'3C} SBC 和'H (l3C} MBC 光谱是使用布鲁克反向电子器件，使用布鲁克 10 毫米宽带探头收集的。'H {'3C} SBC 光谱是在采集过程中没有 I3C 去耦的情况下记录的；交叉峰显示为由 'JcH（约 140-160 Hz）分隔的双峰。所用的延迟时间为 3.12 ms，以优化 160 Hz'H-I3C 耦合器 用于'H {13C} MBC。
MATERIALS AND METHODSL-lysyl-L-tryptophyl-L-lysine and L-tryptophan were purchased from Sigma Chemical Co., and used without further purification. The tripeptide sample used for nmr spectroscopy was 50 mM L-lysyl-L-tryptophyl-L-lysine dissolved in 2.8 mL'H, O containing 100 mM phosphate buffer at pH* 7.24 (pH reading uncorrected for deuterium isotope effect). The free amino acid sample was 28 mM L-tryptophan dissolved in dimethylsulfoxide (DMSO-d,). All nmr data were collected at 25 C on a Bruker AM-400 WB nmr spectrometer operating at a'H frequency of 400.13 MHz and a I3C frequency of 100.6 MHz. The'H {'3C} SBC and'H (l3C} MBC spectra were collected with a Bruker 10-mm broad-band probe by using Bruker reverse electronics. The'H {'3C} SBC spectrum was recorded without I3C decoupling during acquisition; the cross peaks appear as doublets separated by'JcH (ca. 140-160 Hz). The delay time used was 3.12 ms to optimize for 160 Hz'H-I3C couplings. For the'H {13C} MBC