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利用液相色谱-质谱联用技术分析了Keggin型12-磷钨酸化学转化人参皂苷Rb1产物的结构与转化途径.基于高效液相色谱对转化产物的快速分离,利用Q Exactive高分辨质谱的Full MS-AIF模式快速鉴定了产物结构,并利用多级串联质谱进行结构验证.进一步结合人参皂苷异构体在反向C18色谱柱上的相对保留时间,快速分析鉴定出Rb1的10种转化产物为20(S)-Rg3,20(R)-Rg3,20(S)-25-OH-Rg3,20(R)-25-OH-Rg3,25-OH-Rk1,25-OH-Rg5,Rg5,Rk1,(20S,25)-环氧-Rg3和(20R,25)-环氧-Rg3.根据转化产物的结构初步推断了人参皂苷的转化途径:在12-磷钨酸产生的酸性环境中,Rb1主要通过C20位去糖基化、差向异构化和烯烃链的水合、消除及环合反应转化为稀有皂苷.采用三重四极杆质谱的选择反应监测模式准确定量分析了Rb1的转化效率和稀有皂苷20(S)-Rg3,20(R)-Rg3,Rk1和Rg5的产率.定量分析结果显示,与生物转化相比,12-磷钨酸对Rb1有更高的转化效率,反应40 min后转化率达到100%.本文结果表明,HPLC-HRMS/MSn/Qq Q技术是人参皂苷等天然产物结构解析与定量分析的有效方法. 相似文献
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使用超越平均场Skyrme-Hartree-Fock(SHF)模型对∧9Be,∧∧10Be,∧13C和∧21Ne进行计算,采用SLy4参数组的Skyrme力作为NN相互作用力,采用最近提出的SLL4参数组的Skyrme力作为N∧相互作用。计算中包含了超子的自旋-轨道力以再现单粒子态的自旋-轨道能级分裂和不交叉效应,并采用BCS方法处理对力。讨论了不同组态超核的相关性质,包含12C⊗∧[000]1/2+,12C⊗∧[110]1/2-,12C⊗∧[101]3/2-和12C⊗∧[101]1/2-及8Be⊗∧[000]1/2+,8Be⊗∧[110]1/2-,8Be⊗∧[101]3/2-和8Be⊗∧[101]1/2-。计算了∧9Be,∧13C的低激发能谱并与实验值进行了比较。结果表明,采用的超越平均场SHF模型能很好地再现∧超子占据s∧轨道的正宇称能级。对8Be的计算结果表明该模型可以很好地再现8Be的集团结构,可以得出∧9Be的真实超核态能级和9Be类似态。对∧9Be及∧13C的计算均再现了自旋双重态(3/2+,5/2+),但是得到的双重态能级差依然与实验值有出入。此外,对于上述超核体系均在∧超子占据∧[000]1/2+轨道时产生了收缩效应。还对∧21Ne进行了计算并和超越平均场RMF模型计算结果进行比较,发现两者计算结果虽有细节上的出入,但是结果基本一致。The beyond-mean-field Skyrme-Hartree-Fock approach is adopted to investigate the properties of ∧9Be, ∧∧10Be, ∧13C and ∧21Ne. The nucleon-nucleon (NN) interaction SLy4 and the nucleon-hyperon(N∧) interaction Skyrme-type SLL4 are used. The spin-orbit force of hyperon is included to show the spin-orbit splitting and non-crossing effect with BCS method to deal with pairing force. Energies of different configurations, such as 12C⊗∧[000]1/2+, 12C⊗∧[110]1/2-, 12C⊗∧[101]3/2-, 12C⊗∧[101]1/2-, 8Be⊗∧[000]1/2+, 8Be⊗∧[110]1/2-, 8 Be⊗∧[101]3/2- and 8Be⊗∧[101]1/2- are given and used to study the effects of ∧ occupying different orbitals. The calculated energy spectra, including both positive-and negative-parity levels, are given and compared to the experimental data. The observed positive-parity spin-doublet (3/2+,5/2+) are successfully reproduced, but the energy difference needs further investigation. The two well known band structures corresponding to the genuine hypernuclear states and the 9Be-analog states are also obtained and compared with the observed ones. The shrinkage effect of ∧ occupying ∧[000]1/2+ is investigated through the density distributions of nuclear core. And finally the calculation results of ∧21Ne are given and compared with the results of RMF method, which are nearly the same but with differences in some details. 相似文献
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