RESOLUTION OF PHOSPHOLIPID MOLECULAR-SPECIES BY P-31 NMR
RESOLUTION OF PHOSPHOLIPID MOLECULAR-SPECIES BY P-31 NMR
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DOI：
10.1002/mrm.1910290603
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发表时间：
1993-06-01
影响因子：
3.3
通讯作者：
KOMOROSKI, RA
中科院分区：
文献类型：
--
作者：
PEARCE, JM;KOMOROSKI, RA
磷-31核磁共振化学位移的磷脂（PLs）溶解在胆汁盐中的酰基取代基的结构的变化进行了研究。磷脂酰胆碱（PC），磷脂酰乙醇胺（PE），磷脂酰甘油（PG）和磷脂酸（PA）的酰基链中的双键的存在下诱导小，但一致的上场位移相对于相应的二饱和酰基PL信号。不饱和相关的高场位移的幅度约为脱氧胆酸钠胆酸钠的两倍。PC，PE和PG二棕榈酰-二油酰物种对的化学位移分离在较低的温度下略有增加。PC物质对的分辨率最大化，并且在2%胆酸盐中大于约100的值下几乎不依赖于胆酸盐与PL的比率。只有PA物种的分辨率显着变化的pH范围6.5至9.5，在其pK 2附近。位移差异的同源系列的二饱和酰基PC链长度呈对数依赖性。各种PC标准品的光谱用于解释来自蛋黄提取物、大豆提取物和整个人羊水的复合PC信号。P-31 NMR分析与已发表的色谱研究一致。在胆酸盐体系中的复合PL信号的解释是简化的混合物具有有限的酰基链长度和不饱和度。
Phosphorus-31 NMR chemical shifts of phospholipids (PLs) solubilized in bile salts were studied with respect to variations in the structure of the acyl substituents. The presence of double bonds in the acyl chains of phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidylglycerol (PG), and phosphatidic acid (PA) induced small but consistent up-field shifts relative to the corresponding disaturated acyl PL signals. The magnitudes of the unsaturation-related upfield shifts were approximately twice as large in sodium cholate as in sodium deoxycholate. Chemical shift separations of PC, PE, and PG dipalmitoyl-dioleoyl species pairs increased slightly at lower temperatures. Resolution of the PC species pair was maximized and nearly independent of cholate-to-PL ratio at values greater than about 100 in 2% cholate. Only the PA species resolution varied significantly over the pH range 6.5 to 9.5, in the vicinity of its pK2. Shift differences for a homologous series of disaturated acyl PCs showed a logarithmic dependence on chain length. Spectra for a variety of PC standards were used to interpret the composite PC signals from egg yolk extract, soybean extract and whole human amniotic fluid. The P-31 NMR analyses were consistent with published chromatographic studies. Interpretation of composite PL signals in the cholate system is simplified for mixtures having restricted acyl chain length and degree of unsaturation.