Method for extracting compound of phenolic acid from leaves of woodbind
A technology for honeysuckle leaves and plant leaves, which is applied in the field of chlorogenic acid and isochlorogenic acid, can solve the problems affecting the extraction and separation of chlorogenic acid and isochlorogenic acid, and achieves low cost, reduced production cost and simple process operation. Effect
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Embodiment 1
[0031] 1 content determination method
[0032]Instruments and reagents High performance liquid chromatography Aglientl100 series, binary pump G1312A, autosampler, diode array detector, Chemstation A.06.01 chemical workstation, chromatographic column: Aglient Zorbax 80A, Extend-C18 (4.6mm×250mm, 5cm ), experimental water (Guangzhou Robust Food and Beverage Co., Ltd.), acetonitrile is chromatographically pure, and phosphoric acid is analytically pure.
[0033] Chromatographic conditions Mobile phase: 0.2% phosphoric acid solution-acetonitrile (88:12), maintain 0-12min, change the mobile phase ratio linearly to (83:17) in 12-15min, maintain the ratio (83:17) in 15-30min; 30-60min linear change to (50:50). The flow rate is 1.0mL·min -1 , the detection wavelength is 327nm, and the column temperature is 30°C.
[0034] 2 Selection of medicinal materials
[0035] Among the Lonicera plants, honeysuckle gray felt, red glandular honeysuckle (L.hypoglauca), mountain silver flower (L.c...
Embodiment 2
[0075]Take 20kg of the medicinal material of Lonicerae pilosula Lonicerae, grind it into 40 mesh powder, extract petroleum ether at 80°C for 6 hours by Soxhlet method and degrease, then extract 60% ethanol with 8 times the volume of the medicinal material weight, and extract twice under reflux at 85°C, each time 1 Hour. The extracts were combined, and the solvent was recovered under reduced pressure. The resulting concentrated solution was segmented through D101 macroporous resin, and firstly eluted with water, then eluted with 10% and 35% ethanol in sequence. Combine water and 10% alcohol eluate, after concentration, first add ethanol until the alcohol content is 50%, ethanol precipitation, remove the precipitate, concentrate the filtrate to (70°C) relative density 1.08, then add ethanol to the alcohol content 80%, alcohol precipitation, centrifugation to take the supernatant, concentration and vacuum drying to obtain 1.30 kg of crude chlorogenic acid with a purity of 70.3%....
Embodiment 3
[0079] Take 30 kg of Lonicerae pilosula Lonicerae medicinal material, crush it into 40-mesh powder, extract it with petroleum ether at 85° C. for 5 hours by Soxhlet method for degreasing, and extract it twice with 75% ethanol with 10 times the volume of the weight of the medicinal material under heat reflux for 1 hour each time. The solvent was recovered from the extract under reduced pressure, the concentrated solution was separated by D101 macroporous resin, eluted directly with 10% ethanol, and the 10% ethanol eluate was collected; then eluted with 40% ethanol, and the 40% ethanol eluate was collected. Take 10% ethanol eluate, after concentration, first add ethanol until the alcohol content is 50%, ethanol precipitation, remove the precipitate, concentrate the filtrate to (70°C) relative density about 1.10, then add ethanol until the alcohol content is 80% %, precipitated with alcohol, centrifuged to take the supernatant, concentrated and vacuum-dried to obtain 1.9 kg of cru...
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