Katsura Shinji, Furuishi Takayuki, Ueda Haruhisa, Yonemochi Etsuo
School of Pharmacy and Pharmaceutical Sciences, Hoshi University, 2-4-41 Ebara, Shinagawa-ku, Tokyo 142-8501, Japan.
Formulation Research Laboratory, Taiho Pharmaceutical Co., Ltd., 224-2, Ebisuno, Hiraishi, Kawauchi-cho, Tokushima 771-0194, Japan.
ACS Omega. 2021 Jan 4;6(1):533-543. doi: 10.1021/acsomega.0c05016. eCollection 2021 Jan 12.
Using bovine pancreatic ribonuclease A (RNase A) and cholesterol, we synthesized cholesteryl-conjugated ribonuclease A (CHRNase A) to evaluate the influence of a conjugated hydrophobic moiety on protein function. Nuclear magnetic resonance and matrix-assisted laser desorption/ionization time-of-flight spectrometry suggested that one cholesteryl group was conjugated to RNase A. Differential scanning calorimetry indicated that CHRNase A was denatured in the solid state but was folded in phosphate buffer (0.05 mol/L, pH 6.5). CHRNase A resembled RNase A in its secondary structure, but circular dichroism (CD) spectra revealed that the helical content of CHRNase A was decreased and the tertiary structure of CHRNase A differed from that of RNase A. Furthermore, fluorescence measurements, CD spectra, an 8-anilino-1-naphthalenesulfonic acid ammonium salt-based assay, and surface tension measurements suggested that cholesterol was conjugated to a tyrosine residue on the protein surface. The relative activity of CHRNase A to RNase A was 79 ± 7%, and the enzyme activity of CHRNase A by adding β-cyclodextrin (β-CyD) increased to 129 ± 7%. Therefore, we considered that the cholesteryl group interacted with substrate (cytidine 2'3'-cyclic monophosphate monosodium salt) to inhibit the enzyme reaction. Finally, the environment around tyrosine residues in CHRNase A in dimethyl sulfoxide was similar to that of native RNase A in phosphate buffer (0.05 mol/L, pH 6.5). These results suggest that cholesterol conjugation to RNase A altered RNase A functionality, including improvement of RNase A resistance to dimethyl sulfoxide and modulation of the ability of β-CyD to control RNase A enzymatic activity.
我们使用牛胰核糖核酸酶A(RNase A)和胆固醇合成了胆固醇共轭核糖核酸酶A(CHRNase A),以评估共轭疏水部分对蛋白质功能的影响。核磁共振和基质辅助激光解吸/电离飞行时间光谱表明,一个胆固醇基团与RNase A共轭。差示扫描量热法表明,CHRNase A在固态下变性,但在磷酸盐缓冲液(0.05 mol/L,pH 6.5)中折叠。CHRNase A的二级结构与RNase A相似,但圆二色性(CD)光谱显示,CHRNase A的螺旋含量降低,三级结构与RNase A不同。此外,荧光测量、CD光谱、基于8-苯胺基-1-萘磺酸铵盐的测定和表面张力测量表明,胆固醇与蛋白质表面的酪氨酸残基共轭。CHRNase A相对于RNase A的相对活性为79±7%,添加β-环糊精(β-CyD)后CHRNase A的酶活性增加到129±7%。因此,我们认为胆固醇基团与底物(胞苷2'3'-环单磷酸单钠盐)相互作用以抑制酶反应。最后,CHRNase A在二甲基亚砜中的酪氨酸残基周围环境与天然RNase A在磷酸盐缓冲液(0.05 mol/L,pH 6.5)中的环境相似。这些结果表明,胆固醇与RNase A的共轭改变了RNase A的功能,包括提高RNase A对二甲基亚砜的抗性以及调节β-CyD控制RNase A酶活性的能力。