以姜黄素和碘甲烷为原料,一步合成了二甲基姜黄素分子探针L,其结构经X-射线单晶衍射、~1H NMR,~(13)C NMR和ESI-MS等分析手段确证。该化合物晶体属单斜晶系,空间群C2/c,晶胞参数:a=22.317(6)nm,b=8.703 8(19)nm,c=23.039(5)nm,β=93.378(10)°,V=4 467.4(18)nm3,Z=4,Dc=1.206 g·cm-3,F(000)=1 720,μ(MoKα)=0.088 mm-1,R=0.080 9,ωR=0.216 3。探针L在甲醇-水溶液(体积比9∶1,Tris-HCl缓冲溶液,p H 7.2)中对Fe~(3+)具有选择性识别和较强的抗干扰能力。通过紫外滴定以及质谱确证探针L与Fe~(3+)形成1∶1配合物,结合常数(K)为1.089×106L/mol。该识别体系在Fe~(3+)浓度为5.5×10-6~3×10~(-5)mol/L范围内具有较好的线性关系(r2=0.997 8),检出限为2.2×10~(-6)mol/L。
Abstract: The di-O-methylcurcumin L as a molecular probe was directly synthesized by using curcumin and iodomethane. The title compound was characterized by X-ray single-crystal diffraction, t H NMR, 13 C NMR and ESI - MS. The crystal structure of the compound belongs to monoclinic system with a space group of C2/c. The cell parameters were as follows: a = 22. 317 (6) nm, b = 8. 703 8 (19) urn, c = 23.039(5) nm, /3=93.378(10)°, V=4467.4(18) nm3, Z=4, Dc =1.206g.cm-3, F(000) = 1 720, μ (MoKα) = 0. 088 rmn R = 0. 080 9, wR = 0. 216 3. The probe L exhibited a selective and sensitive absorption response toward Fe3+ over a wide range of metal ions in ethanol - water solution (9 : 1, Tris - HC1 buffer, pH 7.2). The results of ultraviolet titration and mass spectrometry showed that the probe L and Fe3 + formed a 1 : 1 complex, and the association constant K was deter- mined to be 1. 089 x 106 L/tool. The mothod showed good linearity(r2 = 0. 997 8) for Fe3+ coneon- tration in the range of 5.5×10-6- 3 × 10-5 mol/L with a limit of detection of 2.2 ×10-6 mol/L.