HIGH-RESOLUTION PROTON AND C-13 NMR OF MEMBRANES - WHY SONICATE

HIGH-RESOLUTION PROTON AND C-13 NMR OF MEMBRANES - WHY SONICATE
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DOI:
10.1021/bi00396a009
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发表时间:
1987-11-03
期刊:
影响因子:
2.9
通讯作者:
FORBES, J
FORBES, J
中科院分区:
生物学3区
文献类型:
--
作者:
OLDFIELD, E;BOWERS, JL;FORBES, J

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我们使用“魔角”样品旋转 (MASS) 技术获得了鸡蛋卵磷脂和鸡蛋卵磷脂-胆固醇 (1:1) 多层的高场 (11.7-T) 质子和碳 13 傅里叶变换 (FT) 核磁共振 (NMR) 谱,并使用传统的 FT NMR 方法获得了超声处理的鸡蛋卵磷脂和鸡蛋卵磷脂-胆固醇 (1:1) 囊泡。纯鸡蛋卵磷脂样品的质子和碳 13 MASS NMR 谱的分辨率与超声处理样品的分辨率基本相同,但使用 MASS 可以比使用更稀释的超声处理系统更快地获得未超声处理的脂质谱。对于 1:1 卵磷脂-胆固醇系统,质子 MASS NMR 光谱实际上与超声处理样品的传统 FT 光谱相同,而使用 13C NMR,我们证明可以监测胆固醇部分中的大多数 13C 核,即使这些相同的核在相应的超声处理系统中基本上是不可见的,即严重展宽。此外,由于浓度效应,13C MASS NMR 谱的记录速度比超声处理样品的记录速度要快得多。总而言之,这些结果强烈表明,未来很少需要诉诸脂质双层膜的超声波破碎来获得高分辨率质子或碳 13 NMR 谱。
We have obtained high-field (11.7-T) proton and carbon-13 Fourier transform (FT) nuclear magnetic resonance (NMR) spectra of egg lecithin and egg lecithin-cholesterol (1:1) multibilayers, using "magic-angle" sample spinning (MASS) techniques, and sonicated egg lecithin and egg lecithin-cholesterol (1:1) vesicles, using conventional FT NMR methods. Resolution of the proton and carbon-13 MASS NMR spectra of the pure egg lecithin samples is essentially identical with that of sonicated samples, but spectra of the unsonicated lipid, using MASS, can be obtained very much faster than with the more dilute, sonicated systems. With the 1:1 lecithin-cholesterol systems, proton MASS NMR spectra are virtually identical with conventional FT spectra of sonicated samples, while with 13C NMR, we demonstrate that most 13C nuclei in the cholesterol moiety can be monitored, even though these same nuclei are essentially invisible, i.e., are severely broadened, in the corresponding sonicated systems. In addition, 13C MASS NMR spectra can again be recorded much faster than with sonicated samples, due to concentration effects. Taken together, these results strongly suggest there will seldom be need in the future to resort to ultrasonic disruption of lipid bilayer membranes in order to obtain high-resolution proton or carbon-13 NMR spectra.