The configurations of C-20 in derivatives of novel 5α-adynerin type,co-existing glycoside in pair,were identified with the calculated chemical shifts of carbon at the B3LYP/6-311＋G（2d,p）level.These glycosides are ...The configurations of C-20 in derivatives of novel 5α-adynerin type,co-existing glycoside in pair,were identified with the calculated chemical shifts of carbon at the B3LYP/6-311＋G（2d,p）level.These glycosides are unusual cardic aglycones without the common olefin bond in ring E.展开更多
[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in bl...[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in blood. The blood sample was dispersed and fixed on a solid phase supported liquid-liquid extraction column and eluted with ethyl acetate. The resulting eluent was used for chromatographic separation with Kinetex C_(18) column as the separation column and gradient elution was performed using 10 mmol/L ammonium formate solution containing 0. 1%( volume fraction) formic acid and acetonitrile as the mobile phase. In the tandem mass spectrometry analysis,the detection was carried out using the electrospray positive ion source multiple reaction monitoring mode. [Results] The mass concentration of oleandrin and adynerin showed linear relationship in the range of 2-100 μg/L. The limit of detection( 3 S/N) of the method was 0. 5 μg/L.A blank sample was used as the substrate for the spike recovery test. The recovery rate was in the range of 90. 0%-98. 0%,and the relative standard deviation( RSD) of the measured values( n = 6) was in the range of 2. 1%-7. 3%. [Conclusions]The method established in this experiment has the benefits of simple pretreatment,good recovery,high sensitivity and strong specificity,and is expected to provide an ideal method for the determination of such drugs in blood.展开更多
A new 5α-adynerin-type cardenolide,named funingenoside U（1）,together with its aglycone,（17R）-3β-hydroxy-4β-acetoxy-8, 14β-epoxy-5α-card-20（22）-enolide,was isolated from the roots of Parepigynumfuningense.Th...A new 5α-adynerin-type cardenolide,named funingenoside U（1）,together with its aglycone,（17R）-3β-hydroxy-4β-acetoxy-8, 14β-epoxy-5α-card-20（22）-enolide,was isolated from the roots of Parepigynumfuningense.Their structures were established on the basis of spectral（MS,1D and 2D NMR） measurements and chemical evidences.展开更多
基金Supported by the Hundred Talents Program of Chinese Academic of Sciences the Science and Technology Committee ofYunnan Province,China.
文摘The configurations of C-20 in derivatives of novel 5α-adynerin type,co-existing glycoside in pair,were identified with the calculated chemical shifts of carbon at the B3LYP/6-311＋G（2d,p）level.These glycosides are unusual cardic aglycones without the common olefin bond in ring E.
基金Supported by Project of National Natural Science Foundation(81273346)
文摘[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in blood. The blood sample was dispersed and fixed on a solid phase supported liquid-liquid extraction column and eluted with ethyl acetate. The resulting eluent was used for chromatographic separation with Kinetex C_(18) column as the separation column and gradient elution was performed using 10 mmol/L ammonium formate solution containing 0. 1%( volume fraction) formic acid and acetonitrile as the mobile phase. In the tandem mass spectrometry analysis,the detection was carried out using the electrospray positive ion source multiple reaction monitoring mode. [Results] The mass concentration of oleandrin and adynerin showed linear relationship in the range of 2-100 μg/L. The limit of detection( 3 S/N) of the method was 0. 5 μg/L.A blank sample was used as the substrate for the spike recovery test. The recovery rate was in the range of 90. 0%-98. 0%,and the relative standard deviation( RSD) of the measured values( n = 6) was in the range of 2. 1%-7. 3%. [Conclusions]The method established in this experiment has the benefits of simple pretreatment,good recovery,high sensitivity and strong specificity,and is expected to provide an ideal method for the determination of such drugs in blood.
文摘A new 5α-adynerin-type cardenolide,named funingenoside U（1）,together with its aglycone,（17R）-3β-hydroxy-4β-acetoxy-8, 14β-epoxy-5α-card-20（22）-enolide,was isolated from the roots of Parepigynumfuningense.Their structures were established on the basis of spectral（MS,1D and 2D NMR） measurements and chemical evidences.
