Viburnum sargentii branch and leaf lignan, extraction method and application
A technology of agarwood and its extraction method, which is applied in the field of natural products, can solve the problem of not being able to obtain the anti-atherosclerotic activity of high-purity agarwood compound monomers, and achieve less pollution and clear structure Effect
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Embodiment 1
[0046] After crushing 20Kg of dried branches and leaves of Qionghua Tianmu, cold-soak in 50L of 95% ethanol at room temperature for 48-72 hours for percolation extraction. The ethanol extract is concentrated under reduced pressure with a 30L large-scale rotary evaporator, and the evaporated ethanol is poured back into the percolation jar for cold soaking 24 to 48 hours; carry out second percolation extraction on the medicinal powder, second concentration, pour the evaporated ethanol back into the percolation tank for cold soaking for 24 to 48 hours; perform third percolation extraction on the medicinal powder, three times of concentration, and recover ethanol , until the concentrated solution has no alcohol smell, 2000g of total extract is obtained, and ethanol is recovered. Suspend the extract in warm water with a constant temperature ultrasonic instrument, sequentially extract with 1 to 1.5 times of petroleum ether, chloroform, ethyl acetate and n-butanol, and concentrate und...
Embodiment 3
[0050] The structure determination of embodiment 3 monomer magnolanin (compound 1)
[0051] White powder (chloroform). ESI-MS m / z: 417[M+H]+, the molecular formula is C 23 h 28 o 7 . 1H-NMR (400MHz, CDCl 3 )δ: 3.10(2H,m,H-1,5),3.82,3.86,3.88(each,3H,s,OMe),3.86(6H,s,OMe),3.92,4.27(each 2H,m,H -4,8); 4.74(2H,m,H-2,6),6.81-6.90(5H,m,Ar-H).13C-NMR(100MHz,CDCl3)δ:54.3(C-1),54.6 (C-5), 56.1(OMe), 56.4(OMe), 61.2(OMe), 72.0(C-4), 72.2(C-8), 85.9(C-2), 86.3(C-6), 103.0 (C-2″,6″),109.4(C-2′),111.2(C-5′),118.5(C-6′),133.6(C-1′),137.0(C-1″), 137.7 (C-4″), 148.9 (C-3′), 149.4 (C-4′), 153.7 (C-3″, 5″). For the hydrogen spectrum and carbon spectrum, please refer to the appendix of the manual figure 2 with image 3
Embodiment 4
[0052] The structure determination of embodiment 4 monomer (+)-cineole (compound 2)
[0053] White powder (chloroform). ESI-MS m / z:387[M+H]+, molecular formula is C 22 h 26 o 6 . 1H-NMR (400MHz, CDCl 3 )δ:6.90-6.80(6H,m,Ar-H),3.10(2H,m,H-1,5),4.74(2H,d,J=4.1Hz,H-2,6),4.25(2H ,dd,J=8.9,6.9Hz,H-4α,8α),3.95(2H,dd,J=8.9,6.9HzH-4β,8β),3.88(6H,s,OCH3×2),3.86(6H, s, OCH3×2),; 13C-NMR (CDCl3, 100MHz) δ: 54.4 (C-1,5), 86.0 (C-2,6), 71.9 (C-4,8), 134.6 (C-1 ′,1″),110.9(C-2′,2″),149.5(C-3′,3″),149.7(C-4′,4″),112.3(C-5′,5″), 119.3 (C-6′,6″), 56.1 (OCH3×2), 56.2 (OCH3×2). For the hydrogen spectrum and carbon spectrum, please refer to the appendix of the manual Figure 4 with Figure 5 .
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