Dibenzocyclooctenes lignans, and preparation method and application thereof
A technology of lignans and semi-preparative chromatography, which is applied in the field of tobacco additives to achieve the effect of improving the quality of cigarettes, the preparation method is simple and easy to operate, and the effect of scavenging free radicals and antioxidant activity
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Embodiment 1
[0024] - Compound preparation
[0025] The cane samples of Schisandra chinensis were collected in Mount Maer, Heqing, Dali, Yunnan. The samples were crushed and passed through a 30-mesh sieve. 3.0 kg of samples were extracted with 70% methanol ultrasonically for three times. g. The extract was dissolved with an appropriate amount of acetone, and then mixed with 250 g of crude silica gel (80-100 mesh), and 2.0 kg of silica gel (160-200 mesh) was packed into a column for silica gel column chromatography, chloroform:methanol (1:0 → 0:1) Gradient elution, TLC monitoring Merge the same fractions to obtain 8 fractions (pure chloroform, chloroform-methanol 20:1, chloroform-methanol 9:1, chloroform-methanol 8:2, chloroform-methanol 3:2, chloroform-methanol 1:1, chloroform-methanol 1:2), in which 15.4 g of chloroform-methanol (9:1) eluted part was separated by Agilent 1100 semi-preparative high-performance liquid chromatography, with 45% methanol as mobile phase, Zorbax SB -C 18 (2...
Embodiment 2
[0027] - identification of compounds
[0028] The patent compound is light yellow colloidal substance; UV spectrum (solvent is methanol), lambda max (log ε ) 320 (2.22), 241 (3.18), 210 (4.26) nm; FTIR (KBr pellet) ν max 3450, 3032, 2876, 2858, 1647, 1587, 1476, 1387, 1154, 1038, 922, 839 cm -1 ; HRESIMS gives quasi-molecular ion peak m / z 405.1918 [M+H] + (calculated value 405.1913). combine 1 H and 13 C NMR spectrum gives a molecular formula C 22 h 28 o 7 , with an unsaturation of 9. From 1 H and 13 C NMR spectrum signal (Figure-1 and Figure-2, see Table-1 for data attribution) It can be seen that there are 2 benzene rings in the compound (including 2 double-bonded methine carbons, δ C 104.4, 107.2), 2 methines ( δ C 37.6, 39.5), 1 oxidized methylene ( δ C 80.5), 1 methylene ( δ C 39.0), 2 methyl groups ( δ C 13.0, 21.8, its hydrogen spectrum is split into double peaks). Combined with the above analysis, it can be determined that this co...
Embodiment 3
[0031] ——Detection of compound antioxidant activity
[0032] Antioxidant activity is expressed by the ability to scavenge DPPH free radicals; 50 μg / mL was used as the initial screening concentration to measure the activity of scavenging lipid free radicals DPPH. Take a costar 96-well plate and add freshly prepared DPPH ethanol solution (6.5×10 5 mol / L) 190 μL / well, add 10 μL / well of the sample to be tested, add 10 μL of normal saline to the blank well, mix well, seal the plate with a sealing film, and keep it at room temperature for 30 minutes in the dark, and measure it under UV2401 spectrophotometry Measure the absorbance value of each hole on the measuring instrument on the meter, and the measurement wavelength is 517 nm; the scavenging rate of the sample to the lipid free radical DPPH is calculated as follows:
[0033] DPPH clearance (%) = (A空白 -A 样品 ) / A 空白 ×100%
[0034] A 空白 : Absorbance value of the blank control group; A 样品 : Add the absorbance value of...
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