Kubalek E W, Kornberg R D, Darst S A
Beckman Laboratories, Fairchild Center, Department of Cell Biology, Stanford University, School of Medicine, CA 94305.
Ultramicroscopy. 1991 Jun;35(3-4):295-304. doi: 10.1016/0304-3991(91)90082-h.
Electron crystallographic analysis of two-dimensional crystals grown on lipid layers at the air/water interface has been limited by loss or damage during transfer of the crystals to an electron microscope support grid. Two methods of transfer are described which are applicable on a small scale (10 microliters of protein solution) and which give greatly improved results for streptavidin crystals on biotinylated lipid layers. In the first method, a hydrophobic grid surface was produced by coating a carbon support film with a thin layer of SiO2, followed by alkylation with dimethyloctadecylchlorosilane. The transfer efficiency of protein crystals approached 50% coverage of the alkylated grid surface. The degree of order of crystals transferred to the alkylated grid surface and preserved in negative stain was significantly improved over that of crystals transferred directly to a carbon support film. In the second method, crystals at the air/water interface were transferred to a holey carbon support film. The efficiency of transfer across the holes was virtually 100% as nearly every hole was completely covered with crystals. After preservation of the crystals in 1% glucose and cooling to liquid nitrogen temperature, electron diffraction was obtained that extended to 1/2.8 A-1 resolution. This demonstrates that two-dimensional crystals grown on lipid layers at the air/water interface can be sufficiently well-ordered, even after transfer to a support grid, to yield high-resolution structural information.
对在空气/水界面的脂质层上生长的二维晶体进行电子晶体学分析,一直受到晶体转移到电子显微镜支撑网格过程中损失或损坏的限制。本文描述了两种转移方法,它们适用于小规模实验(10微升蛋白质溶液),并且对于生物素化脂质层上的链霉亲和素晶体能产生显著改善的结果。在第一种方法中,通过用一层薄的SiO₂涂覆碳支撑膜,然后用二甲基十八烷基氯硅烷进行烷基化,制备出疏水网格表面。蛋白质晶体的转移效率接近烷基化网格表面覆盖率的50%。转移到烷基化网格表面并保存在负染中的晶体的有序度,比直接转移到碳支撑膜上的晶体有显著提高。在第二种方法中,将空气/水界面的晶体转移到有孔碳支撑膜上。穿过孔的转移效率几乎为100%,因为几乎每个孔都被晶体完全覆盖。在将晶体保存在1%葡萄糖中并冷却至液氮温度后,获得了分辨率达到1/2.8 Å⁻¹的电子衍射图。这表明在空气/水界面的脂质层上生长的二维晶体,即使转移到支撑网格后,仍能具有足够好的有序度,从而产生高分辨率的结构信息。