Hausinger R P, Orme-Johnson W H, Walsh C
Biochemistry. 1985 Mar 26;24(7):1629-33. doi: 10.1021/bi00328a010.
Two chromophores with absorbance maxima at 390 nm (factors 390) have been isolated from oxidized cells of Methanobacterium thermoautotrophicum delta H. The isolation procedure included anion-exchange chromatography of the soluble cofactor pool followed by reverse-phase chromatography. The factor 390 species are novel derivatives of methanogen coenzyme factor 420 in which the 5-deazaflavin 8-hydroxy group is in a phosphodiester linkage to adenosine 5'-phosphate or guanosine 5'-phosphate. The structural assignments were based, in part, on the UV-visible and 1H NMR spectra. In addition, the results from amino acid analysis, phosphate determination, 31P NMR spectroscopy, and fast atom bombardment mass spectrometry were consistent with the proposed structures. Confirmation of the factor 390 structures was made following phosphodiesterase release of the nucleotide monophosphates from factor 420. The nucleotide monophosphates were identified as AMP and GMP by UV-visible spectra and based on elution position by using reverse-phase and anion-exchange high-performance liquid chromatography. The presence of AMP was further demonstrated by using adenylate-5'-phosphate kinase which induced a spectral shift during conversion of the sample to IMP. In addition, the presence of GMP was established by a specific enzymatic assay.
已从嗜热自养甲烷杆菌δH的氧化细胞中分离出两种在390 nm处有最大吸光度的发色团(390因子)。分离过程包括对可溶性辅因子池进行阴离子交换色谱,然后进行反相色谱。390因子是产甲烷辅酶因子420的新型衍生物,其中5-脱氮黄素8-羟基与5'-磷酸腺苷或5'-磷酸鸟苷形成磷酸二酯键。结构归属部分基于紫外可见光谱和1H NMR光谱。此外,氨基酸分析、磷酸盐测定、31P NMR光谱和快原子轰击质谱的结果与所提出的结构一致。在磷酸二酯酶从因子420释放出单磷酸核苷酸后,对390因子的结构进行了确认。通过紫外可见光谱并基于反相和阴离子交换高效液相色谱的洗脱位置,将单磷酸核苷酸鉴定为AMP和GMP。通过使用5'-磷酸腺苷激酶进一步证明了AMP的存在,该激酶在样品转化为IMP的过程中引起光谱位移。此外,通过特定的酶促测定确定了GMP的存在。