Aminophenyl- and nitrophenyl-labeled nucleoside triphosphates:: Synthesis, enzymatic incorporation, and electrochemical detection

Aminophenyl- and nitrophenyl-labeled nucleoside triphosphates:: Synthesis, enzymatic incorporation, and electrochemical detection
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DOI:
10.1002/anie.200705088
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发表时间:
2008-01-01
影响因子:
16.6
通讯作者:
Hocek, Michal
Hocek, Michal
中科院分区:
化学1区
文献类型:
--
作者:
Cahova, Hana;Havran, Ludek;Hocek, Michal

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核磁共振谱在Bruker avance 600(1 H为600 MHz,13 C核为151 MHz)和Bruker 500(1 H为500 MHz,13 C为125.7 MHz,31 P为202.3)D2O中(以二恶烷为内标,δH=3.75ppm,δC=69.3ppm,31P核磁共振的标准为外部磷酸)上测量。化学位移以ppm(δ标度)为单位,耦合常数(J)以赫兹为单位。使用H,HCOSY,H,C-HSQC和H,C-HMBC实验的组合完成了所有核磁共振信号的指定。在LCQ Classic(Thermo-Finnigan)光谱仪上使用ESI或Q-TOF Micro(Waters,ESI源,锁定喷雾内校准)测量质谱图。制备高效液相色谱法,色谱柱为10µm C18反相柱(Phenomeex,露娜C18(2))。
NMR spectra were measured on a Bruker Avance 600 (600 MHz for 1 H and 151 MHz for 13 C nuclei) and a Bruker 500 (500 MHz for 1 H, 125.7 MHz for 13 C and 202.3 for 31 P) in D2O (referenced to dioxane as internal standard, δH= 3.75 ppm, δC= 69.3 ppm, standard for 31 P NMR was external H3PO4). Chemical shifts are given in ppm (δ-scale), coupling constants (J) in Hz. Complete assignment of all NMR signals was performed using a combination of H, HCOSY, H, C-HSQC and H, C-HMBC experiments. Mass spectra were measured on LCQ classic (Thermo-Finnigan) spectrometer using ESI or Q-Tof Micro (Waters, ESI source, internal calibration with lockspray). Preparative HPLC separations were performed on a column packed with 10 µm C18 reversed phase (Phenomenex, Luna C18 (2)).