Nine compounds were isolated from the extract of the roots of Oplopanax elatus Nakai(Echinopanax elatus Nakai),family Araliaceae.The chemical structures of six compounds wereestablished by measuring chemical and physi...Nine compounds were isolated from the extract of the roots of Oplopanax elatus Nakai(Echinopanax elatus Nakai),family Araliaceae.The chemical structures of six compounds wereestablished by measuring chemical and physical constants,spectral data(IR,EI-MS,FD-MS,~1HNMR and ^(13)CNMR)and chemical methods,as 1-heptacosanol,β-sitosterol,daucosterol,展开更多
Using heptane, toluene, and tetrahydrofuran （THF） as eluant, asphaltenes were fractionated into five fractions based on their polarity and solubility. The molecular composition of polar heteroatom species in both as...Using heptane, toluene, and tetrahydrofuran （THF） as eluant, asphaltenes were fractionated into five fractions based on their polarity and solubility. The molecular composition of polar heteroatom species in both asphaltene and its fractions were ana- lyzed by negative-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry （ESI FT-ICR MS）. The application of UV-vis spectrometer in characterizing asphaltene composition and measuring asphaltene concentration was discussed. About 11.9 wt% asphaltene components adsorbed permanently on silica gel in the extrography column after exces- sive elution with various solvents. In negative FT-ICR MS, the mass spectra show that acidic and neutral nitrogen-containing compounds such as N1 and NIS1 mainly existe in the first three less polar fractions, while oxygen-containing compounds such as 02, O2S, O2S2, 03, and 04 show high relative abundance in more polar fractions. These results suggest oxygen-containing compounds have stronger adsorption ability with silica gel. It was observed that the double bond equivalence （DBE） distribu- tion of N1 class species in the fractions shifted to higher values while the carbon number shifted to smaller numbers as polarity of fractions increased. This indicates that acidic and neutral Nl compounds with longer carbon chain and less aromaticity have less polarity compared with those with shorter carbon chain and stronger aromaticity. UV-vis absorbance indicats that fractions containing the most aromatic and most polar asphaltene have better absorbance at long wavelength, while the fractions that consist of least aromatic and least polar asphatlenes show high absorbance at short wavelength.展开更多
Salinomycin sodium（SAL-Na） is a type of antibiotic chemotherapeutic drugs with the potential to treat cancer stem cells. The assay method of SAL-Na included in the pharmacopoeia is a microbiological method, which is...Salinomycin sodium（SAL-Na） is a type of antibiotic chemotherapeutic drugs with the potential to treat cancer stem cells. The assay method of SAL-Na included in the pharmacopoeia is a microbiological method, which is not suitable for the rapid detection in daily scientific research. Besides, the assay methods of SAL-Na reported by literature are not suitable for quantification due to the interference of various excipients. Consequently, the deep study on biological mechanism of SAL-Na is hindered by its assay method. In the present study, we aimed to establish an ultraviolet visible（UV-vis） spectrophotometric method to determine the content of SAL-Na in the liposomes. The first approach was a UV spectrophotometry, in which SAL-Na was dissolved in ethanol and then detected at 287 nm. Although the standard curve measured at 287 nm by UV method had good linearity, the quantification limitation was too high to meet the requirement in determining SAL-Na in the liposomes. In addition, the membrane materials in the liposomes severely affected the measurement. The second one was an improved UV-vis spectrophotometry by vanillin derivatization. In this method, SAL-Na was dissolved in 95% ethanol, mixed with vanillin test solution and heated at 72 ℃ for 40 min for derivatization. After cooling down to room temperature, the solution was detected using UV-vis spectrophotometer at 526 nm. This method could be used to accurately determine the content of SAL-Na at lower concentration, and the absorbance value was stable for 5 d at least. Moreover, the membrane materials of the liposomes did not affect the absorbance of SAL-Na at 526 nm. The precision and recovery studies demonstrated that the vanillin derivatization approach was stable and precise in assaying SAL-Na. In conclusion, the UV-vis spectrophotometry by vanillin derivatization could be used for measuring SAL-Na in the liposomes, thereby laying a foundation for deep study of the biological mechanism of SAL-Na in the liposomes.展开更多
文摘Nine compounds were isolated from the extract of the roots of Oplopanax elatus Nakai(Echinopanax elatus Nakai),family Araliaceae.The chemical structures of six compounds wereestablished by measuring chemical and physical constants,spectral data(IR,EI-MS,FD-MS,~1HNMR and ^(13)CNMR)and chemical methods,as 1-heptacosanol,β-sitosterol,daucosterol,
文摘Using heptane, toluene, and tetrahydrofuran （THF） as eluant, asphaltenes were fractionated into five fractions based on their polarity and solubility. The molecular composition of polar heteroatom species in both asphaltene and its fractions were ana- lyzed by negative-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry （ESI FT-ICR MS）. The application of UV-vis spectrometer in characterizing asphaltene composition and measuring asphaltene concentration was discussed. About 11.9 wt% asphaltene components adsorbed permanently on silica gel in the extrography column after exces- sive elution with various solvents. In negative FT-ICR MS, the mass spectra show that acidic and neutral nitrogen-containing compounds such as N1 and NIS1 mainly existe in the first three less polar fractions, while oxygen-containing compounds such as 02, O2S, O2S2, 03, and 04 show high relative abundance in more polar fractions. These results suggest oxygen-containing compounds have stronger adsorption ability with silica gel. It was observed that the double bond equivalence （DBE） distribu- tion of N1 class species in the fractions shifted to higher values while the carbon number shifted to smaller numbers as polarity of fractions increased. This indicates that acidic and neutral Nl compounds with longer carbon chain and less aromaticity have less polarity compared with those with shorter carbon chain and stronger aromaticity. UV-vis absorbance indicats that fractions containing the most aromatic and most polar asphaltene have better absorbance at long wavelength, while the fractions that consist of least aromatic and least polar asphatlenes show high absorbance at short wavelength.
基金National Science Foundation of China(Grant No.81673367)
文摘Salinomycin sodium（SAL-Na） is a type of antibiotic chemotherapeutic drugs with the potential to treat cancer stem cells. The assay method of SAL-Na included in the pharmacopoeia is a microbiological method, which is not suitable for the rapid detection in daily scientific research. Besides, the assay methods of SAL-Na reported by literature are not suitable for quantification due to the interference of various excipients. Consequently, the deep study on biological mechanism of SAL-Na is hindered by its assay method. In the present study, we aimed to establish an ultraviolet visible（UV-vis） spectrophotometric method to determine the content of SAL-Na in the liposomes. The first approach was a UV spectrophotometry, in which SAL-Na was dissolved in ethanol and then detected at 287 nm. Although the standard curve measured at 287 nm by UV method had good linearity, the quantification limitation was too high to meet the requirement in determining SAL-Na in the liposomes. In addition, the membrane materials in the liposomes severely affected the measurement. The second one was an improved UV-vis spectrophotometry by vanillin derivatization. In this method, SAL-Na was dissolved in 95% ethanol, mixed with vanillin test solution and heated at 72 ℃ for 40 min for derivatization. After cooling down to room temperature, the solution was detected using UV-vis spectrophotometer at 526 nm. This method could be used to accurately determine the content of SAL-Na at lower concentration, and the absorbance value was stable for 5 d at least. Moreover, the membrane materials of the liposomes did not affect the absorbance of SAL-Na at 526 nm. The precision and recovery studies demonstrated that the vanillin derivatization approach was stable and precise in assaying SAL-Na. In conclusion, the UV-vis spectrophotometry by vanillin derivatization could be used for measuring SAL-Na in the liposomes, thereby laying a foundation for deep study of the biological mechanism of SAL-Na in the liposomes.
