Higher value application method for shaddock agricultural waste resource
An agricultural waste, high-value technology, applied in the direction of fermentation, can solve the problems of low supply of trilobatin, high difficulty, poor operability of the refining process, etc., and achieve low cost, high product quality, and environment-friendly. Effect
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Embodiment 1
[0025] Put 250 kg of crushed and dried Shatian pomelo secondary fruit into a 2-ton extraction tank, add 1500 L of 75% ethanol, heat and reflux for 1 hour; filter the material, and repeat the extraction three times. Inject the extract into a 2T hydrogenation reaction tank, add 150 kg of NaOH and 23 kg of commercial Raney nickel as catalysts, vacuumize and replace with nitrogen, repeat 3 times and then introduce hydrogen, the hydrogen pressure is 1 atmosphere. Then hydrogenate at room temperature for 20 hours. After filtering, the filtrate was adjusted to neutrality with hydrochloric acid in a neutralization tank, and the solid was collected by filtration to obtain 200 kg of wet alkaline hydrogenation product of pomelo flavonoids.
Embodiment 2
[0027] Put 7 kg of the wet alkaline hydrogenation product of pomelo flavonoids obtained above into the enzyme reaction tank, add phosphate buffer solution of pH 6.8 and 5 L rhamnosidase, and react at 30 ° C for 12 h under the condition of slow stirring 100 r / min , and then the solution was heated to 80 degrees, adding activated carbon and stirring for 0.5 hours, filtered and frozen for crystallization. Obtain 4 kg of trilobatin crude product, and obtain a refined product with a content of 99% after recrystallization from ethanol water.
[0028] ESI-MS (m / z): 435[(M-1) + ].
[0029] 1 H NMR (300 MHz, (CD 3 ) 2CO) δ: 2.87 (2H, t), 3.32-3.54 (7H, m), 3.67 (m, 1H), 3.87 (1H, d), 4.35 (2H, s), 4.68 (s, 1H), 4.99 ( 1H, d), 6.11 (s, 2H), 6.71 (2H, d), 7.06 (2H, d), 8.09 (1H, s), 12.36 (2H, s).
Embodiment 3
[0031] Put 7 kg of the wet alkaline hydrogenation product of pomelo flavonoids obtained above into a reaction tank, add 20% ethanol water to dissolve, and react with 20 kg of solid rhamnosidase at 60°C for 4 hours. The resulting reaction solution was released, filtered to remove solid matter, and cooled to crystallize to obtain 4.3 kg of trilobatin with a content of 96%.
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