C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051...C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.展开更多
8,2＇-Diprenylquercetin 3-methyl ether with significant anti-breast cancer activity is the main constituent of Tibetan medicine Sinopodophylli Fructus. In the present study, we developed and validated a rapid and sens...8,2＇-Diprenylquercetin 3-methyl ether with significant anti-breast cancer activity is the main constituent of Tibetan medicine Sinopodophylli Fructus. In the present study, we developed and validated a rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for the determination of 8,2＇-diprenylquercetin 3-methyl ether in rat plasma. 8-Prenylkaempferol was used as the internal standard. The separation was carried out using Waters ACQUITY UPLC BEH C18 column （2.1 mm×100 ram, 1.7 μm） with a mobile phase consisting of acetonitrile and 0.1% formic acid in water on a gradient program at a flow rate of 0.4 mL＇min-1 and temperature of 30 ℃. Triple quadrupole mass spectrometric detection in negative ion mode was used for multiple-reaction monitoring of the transitions at m/z 451.30→177.25 and m/z 353.25→298.15 for 8,2＇-diprenylquercetin 3-methyl ether and 8-prenylkaempferol, respectively. The calibration curves were linear within the concentration range 0.1-2000 ng/mL （r = 0.9954）. The recoveries were 103%-115%, and the results were consistent across low, middle and high concentration levels. The intra- and inter-day precisions were within 15%, and the bias was between --6%-15%. This method was simple, rapid and sensitive, which could be applied to the determination of 8,2＇-diprenylquercetin 3-methyl ether in plasma and pharmacokinetic study in rats. Pharmacokinetic test indicated that the peak plasma concentration occurred in 2 h after the female rats were intragastrically administered with 8,2＇-diprenylquercetin 3-methyl ether at the dose of 100 mg/kg, and the biological half-life was 6.79 h. The blood drug concentration maintained equal amount for 20 h, which was conducive to the in vivo effects of drugs.展开更多
文摘C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.
基金National Natural Science Foundation of China(Grant No.81673590)National Key Technology R&D Program "New Drug Innovation" of China(Grant No.2013ZX09103002-006)
文摘8,2＇-Diprenylquercetin 3-methyl ether with significant anti-breast cancer activity is the main constituent of Tibetan medicine Sinopodophylli Fructus. In the present study, we developed and validated a rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for the determination of 8,2＇-diprenylquercetin 3-methyl ether in rat plasma. 8-Prenylkaempferol was used as the internal standard. The separation was carried out using Waters ACQUITY UPLC BEH C18 column （2.1 mm×100 ram, 1.7 μm） with a mobile phase consisting of acetonitrile and 0.1% formic acid in water on a gradient program at a flow rate of 0.4 mL＇min-1 and temperature of 30 ℃. Triple quadrupole mass spectrometric detection in negative ion mode was used for multiple-reaction monitoring of the transitions at m/z 451.30→177.25 and m/z 353.25→298.15 for 8,2＇-diprenylquercetin 3-methyl ether and 8-prenylkaempferol, respectively. The calibration curves were linear within the concentration range 0.1-2000 ng/mL （r = 0.9954）. The recoveries were 103%-115%, and the results were consistent across low, middle and high concentration levels. The intra- and inter-day precisions were within 15%, and the bias was between --6%-15%. This method was simple, rapid and sensitive, which could be applied to the determination of 8,2＇-diprenylquercetin 3-methyl ether in plasma and pharmacokinetic study in rats. Pharmacokinetic test indicated that the peak plasma concentration occurred in 2 h after the female rats were intragastrically administered with 8,2＇-diprenylquercetin 3-methyl ether at the dose of 100 mg/kg, and the biological half-life was 6.79 h. The blood drug concentration maintained equal amount for 20 h, which was conducive to the in vivo effects of drugs.
