基于~1H-NMR、~(31)P-NMR的三苯基膦三间磺酸钠定量分析研究

该文建立了三苯基膦三间磺酸钠(TPPTS)的核磁氢谱(~1H-NMR)、核磁磷谱(~(31)P-NMR)、定量分析方法。通过~1H-NMR、~(13)C-NMR、~(31)P-NMR并结合~1H-~1H COSY、~1H-~(13)C、~1H-~(13)C HMBC对TPPTS的氢原子、碳原子以及磷原子的化学位移进行归属;氢谱定量选用三■烷作内标、氘代N,N-二甲基甲酰胺(DMF-D_7)作溶剂,磷谱定量选用KH_2PO_4作内标、氘代水(D_2O-D_2)作溶剂,通过对混合体系中各自旋核纵向弛豫时间(T1)的测定,为弛豫延迟时间(D1)的合理设置提供依据。以上两种方法对体系中TPPTS的定量分析结果分别为(58.72±0.21)%、(58.51±0.21)%,测定结果一致性高、平行性好,且检测过程无需待测组分的标准品,能实现TPPTS含量的快速准确测定。

Study on Quantitative Analysis of Tris(3 sulfonatophenyl) Phosphine Sodium Salt Hydrate Using 1H-NMR and 31P-NMR

A method based on 1H-NMR and 31P-NMR was established for the quantitative analysis of tris(3 sulfonatophenyl) phosphine sodium salt hydrate(TPPTS).Through one dimensional 1H-NMR,13C-NMR,31P-NMR and two-dimensional 1H-1H COSY,1H-13C HSQC, 1H-13C HMBC,the chemical shift of TPPTS including all the hydrogen atoms,carbon atoms and phosphorus atoms were assigned.Trioxane was selected as the internal standard compound while N,N-dimethylformamide-D7(DMF-D7) was used as solvent in the 1H-NMR test.Correspondingly,KH2PO4 and deuterium oxide(D2O-D2) were used in the 31P-NMR test.The pulse delay time(D1) of the mixing system was set reasonably based on results of the longitudinal relaxation time(T1) test.Quantitative analysis results of TPPTS by 1H-NMR and 31P-NMR were (58.72 ± 0.21)% and (58.51 ± 0.21)%,respectively,which are close and parallel.Meanwhile,there is no need for the standards of the samples to be detected in the process.Thus the rapid and effective determination of TPPTS in the mixing system could be realized.