CN00128226.3 reports a method for industrial production of a high-concentration Lycopene Powder crystalline product with a lycopene content > 10%.
1. Raw material: the raw material that the present invention produces Lycopene Powder adopts has two kinds, and one is tomato sauce, concentration ratio 3～8: 1 (referring to obtain 1 part of tomato sauce by 3～8 parts of fresh tomato), its lycopene The content is 40-70mg/100g, and it is stored in large barrels and used for annual industrial production; the second is the leftovers separated from the beater in the process of tomato paste production—tomato skin dregs, whose main component is tomato skin And tomato seeds, the content of lycopene in tomato skin is about 35mg/100g.
2. Removal of water-soluble components in tomato paste: add 1-5 times of water to the concentrated tomato paste in 1-3 times, stir, and heat to maintain the temperature at 20-70°C, so that the soluble components in tomato paste can be as much as possible Dissolved in water, centrifuged to remove water and soluble substances dissolved in it, such as sugar, organic acid, inorganic salt, pectin, etc., the removed part of the juice is called tomato clear juice, which can be processed for downstream products. Such as concentration, preparation of tomato beverage, etc.; the obtained tomato pulp residue is wet tomato sauce residue, which mainly contains components such as cellulose, oils, carotenoid pigments, etc., and the water content is 80%-90%;
If tomato peels are used as raw materials, since the wet tomato peels discharged from the beater of the tomato paste production line have a water content of 80-93%, they are easy to rot and deteriorate, so the method of drying first and then separating the peels and seeds can be used; Adopt the method of first separating the skin and seeds, and then drying; in the present invention, the method of first separating the skin and seeds, and then drying is adopted. The specific operation is to add 2 to 5 times of water to the wet tomato skin residue, mix and stir evenly, and pump into the hydrocyclone, using the difference in the sedimentation velocity of the tomato skin and seeds to separate the two, and finally the tomato skin is discharged from the upper part of the hydrocyclone, and the tomato seeds are discharged from the bottom of the hydrocyclone; the tomato skin is passed through the centrifuge Remove the moisture attached to it, and then enter the drying equipment for drying, preferably using belt drying equipment for drying, the drying temperature is 50-80°C, the drying time is 0.3-1h, and the tomato skin is dried to a moisture content of 1.0-8.0%.
3. Degreasing treatment of tomato paste residue: add 1 to 3 times the amount of 0.5% to 5% (w/v%) lye in the tomato paste residue, the alkali used is sodium hydroxide, sodium carbonate or other alkaline substances, Keep warm at 20-70°C for 5-30 minutes to dissolve the lipids and other components in the tomato sauce residue, centrifuge to remove the lye, rinse repeatedly with clean water, and centrifuge for 2-3 times. In the present invention, the degreasing treatment may not be used, but the oleoresin content in the lycopene extract is relatively high, which will affect the crystallization process of Lycopene Powder. In the present invention, it is preferred to treat the tomato puree residue with alkali.
4. Drying of tomato paste residue: Various conventional drying equipment can be used to dry tomato paste residue or tomato skin. It is preferred to use paddle-type drying equipment to dry wet tomato residue to a water content of 60%-75%, and then use belt drying Type drying equipment, the drying temperature is 50-80°C, the drying time is 0.5-3h, and the tomato paste residue is dried to a water content of 3.0-12.0%, preferably a water content of 3-5%, and a lycopene content of 150-360mg /100g; cooled to room temperature, bagged and stored at a low temperature below 20°C, preferably at a temperature of 0-5°C, away from light and oxygen; the dried tomato paste residue can be used as lycopene within a certain period of time Production raw material storage; wet tomato paste residue can also be directly used for the extraction of lycopene without drying.
5. Pulverization: On the day of leaching, pulverize the dried tomato sauce residues in dry storage, and sieve to make the particle size 20-60 mesh.
6. Lycopene leaching: the present invention uses organic solvents such as alcohol, solvent gasoline, ethyl acetate, ether, petroleum ether, hexane, acetone, etc. to extract lycopene, and the ratio of solvent to raw material is 1.2 to 5.0:1 , the leaching temperature is 30-75°C, generally 2-7 times of leaching, the single leaching time is 20-60min, and the stirring speed is 1-20 rpm; before the start of leaching, remove the air in the leaching tank It is proposed that the extraction solvent is sucked into the tank by means of the vacuum in the tank; inert gas, such as nitrogen, carbon dioxide, etc., is used for protection during the entire leaching process to prevent the loss of active ingredients;
7. Filter out the lycopene extract and concentrate and crystallize: After the extraction is completed, filter the extract containing lycopene from the extraction tank, and use a high-density filter cloth larger than 200 mesh to filter the extract. Filtration of the lycopene extract is filtered and sent to a flash tank for flash concentration under a pressure of 200-2000Pa to remove more than 2/3 of the organic solvent in the extract, and the extract is concentrated to make the tomato The content of lycopene reaches >150mg/100ml, and at the same time, the temperature of the concentrated extract is rapidly reduced to -25°C~-10°C. At this temperature, the saturated solubility of lycopene is 40~60mg/100ml, which is in a supersaturated state , so lycopene crystallizes out and is sent into the crystallization tank to complete the crystallization;
Lycopene Powder crystallization: In a low-temperature crystallization tank at -5 to 25°C, the >60% lycopene crystals contained in the concentrated extract are precipitated; <200Pa) to obtain a lycopene crystal product with a lycopene content of not less than 10%;
8. The obtained Lycopene Powder crystallization product is stored in a sealed tank filled with inert gas (preferably nitrogen, carbon dioxide); or diluted and dissolved to prepare various types of lycopene products with various required concentrations.
Harvest 3L of B. trispora fermentation liquid, filter the fermentation liquid to obtain 900 g of B. trispora mycelium. The mycelium was mixed with 2L of 95% ethanol and stirred for 30 minutes. Treated mycelium was filtered and separated to obtain 540g wet mycelia and 2.5L ethanol treatment liquid. The wet mycelium was vacuum-dried at 45° C. for 10 hours to obtain 200 g of dried mycelium. Dried mycelium pulverizes 1 hour under 500rpm with ball mill, then crosses 300 mesh sieves, obtains B. trispora mycelium powder sample.
Supercritical CO2 Extraction of Mycelium of B. trispora
The 200g B. trispora mycelium powder sample that is obtained is packed into a barrel in a 2L extractor, and sealed. Start the temperature control system of the supercritical CO2 extractor, the primary separator and the secondary separator, so that the temperatures of the extractor, the primary separator and the secondary separator are 40 ° C, 55 ° C and 30 ° C, and then close the extraction Throttle and pressure reducing valve behind the extractor, start the compression pump, press carbon dioxide into the extractor, when the extractor is boosted to 30Mpa, adjust the throttle and pressure reducing valve behind the extractor, so that the pressure of the primary separator is 12Mpa, The pressure of the secondary separator is cylinder air pressure, and the average flow of CO2 is controlled at 20L/hour. After all the pressure was stabilized, the extraction was circulated for 2 hours. Turn off the temperature control system and the power supply of the compressor pump, depressurize and recover carbon dioxide. The separated extract in the separator was discharged to obtain 82 g of lycopene oleoresin with a lycopene content of 4.5%.
Take 40g of the above-mentioned lycopene oleoresin and fully dissolve it in 50ml of ethyl acetate. After standing for stratification, discard the lower layer and filter to obtain 45ml of ethyl acetate solution with lycopene. Next, 50 ml of absolute ethanol was added to the ethyl acetate solution, and electromagnetically stirred for 3 hours. The crystalline Lycopene Powder was obtained by filtration with a Buchner funnel, the crystals were washed 3 times with absolute ethanol, the crystals were collected and vacuum-dried to obtain 2.1 g of lycopene crystals with a purity of 60%.
