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Method for extracting xanthohumol in hop residue by supercritical CO2 technology
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A technology for hop residue and xanthohumol, which is applied in the field of hops, can solve the problems of high operation cost, low extraction efficiency and high requirements on equipment conditions, and achieves the effects of green process, simple process and good solubility.
Active Publication Date: 2012-04-25
BEIJING YANJING BREWERY +1
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Domestic patents such as CN101337876A, CN101440029A, and CN101433592A all use organic solvents to extract xanthohumol. In 2005, Dr. Xiong Haoping of Zhejiang University reported the paper "Research on Chemical Components of Hops and Purification Technology of Xanthohumol" using supercritical CO 2 The extraction research of xanthohumol in hops is carried out by using advanced technology, but this research only studies the supercritical extraction parameters, and does not mention the separation parameters, and the application of this research to the subsequent purification research of finished products is slightly insufficient, industrial application The prospect is poor, and the extraction efficiency is low; while foreign reports on xanthohumol extraction technology mainly focus on the use of supercritical CO 2 Both extraction (eg CA2451461) and organic solvent extraction (eg US3794744, US6867332, WO2009 / 023710)
In the above studies, the xanthohumol product obtained by extraction with organic solvents may have solvent residues and poor solubility, and the operating environment is poor, which is likely to cause human injury and other problems; while using supercritical CO 2 Reports on extraction technology may have problems such as high equipment requirements and high operating costs
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Embodiment 1
[0052] (1) Put 1000g of 90 type granular hops into the supercritical extraction kettle, install the top cover, increase the pressure of the extraction kettle to 25MPa, the temperature is 45°C, the separation pressure is 5MPa, the temperature is 30°C, and the extraction time is 3 hours. 813 g of hop residue (hop residue) was obtained.
[0053] (2) Weigh 600g of the hop extract residue, of which the mass content of xanthohumol is 0.38%, put it into the extraction kettle, install the top cover, and increase the pressure of the extraction kettle to prepare for extraction; measure 600ml of 95% edible ethanol , Add to the entrainer tank.
[0054] (3) Supercritical CO 2 Extraction conditions: temperature 55℃, pressure 25MPa, flow acceleration of the entrainer pump 0.6L / hour, CO 2 The flow rate is 14L / hour, the separation temperature is 50°C, the pressure is 10MPa, and the extraction time is 4 hours.
[0055] (4) When the pressure and temperature reach the working state, turn on the entrain...
Embodiment 2
[0061] (1) Put 1000g of 90 type granular hops into the supercritical extraction kettle, install the top cover, increase the pressure of the extraction kettle to 25MPa, the temperature is 45°C, the separation pressure is 5MPa, the temperature is 30°C, and the extraction time is 3 hours. 824 g of the hop residue (hop residue) was obtained.
[0062] (2) Weigh 600g of the hop extract residue, in which the mass content of xanthohumol is 0.38%; Measure 600ml of 95% edible ethanol, mix it with the hop extract residue evenly, put it into the extraction kettle, and install the top cover , The extraction kettle is pressurized and ready for extraction.
[0063] (3) Supercritical CO 2 Extraction conditions: temperature 50℃, pressure 30MPa, CO 2 The flow rate is 18L / hour, the separation temperature is 45°C, the pressure is 5MPa, and the extraction time is 3 hours.
[0064] (4) When the pressure and temperature reach the working state, start timing.
[0065] (5) After the extraction, 560 ml of a d...
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Abstract
The invention discloses a method for extracting xanthohumol in hop residue by supercritical CO2 technology, and relates to the hop technology. The method comprises the following steps: taking raffinate (the hop residue) after alpha acid is extracted from hop by supercritical CO2 as a main raw material, adopting the supercritical CO2 technology, taking ethanol or methanol as an entrainer, and obtaining coarse xanthohumol; performing concentration and spray drying to obtain a coarse product of xanthohumol; and purifying to obtain a high-purity xanthohumol product. The method utilizes the raffinate after alpha acid is extracted from hop by supercritical CO2, and belongs to resource recycling. The method has simple process; the obtained xanthohumol product has good characteristics of high activity and good dissolubility; and the technological process is environment-friendly.
Description
Technical field [0001] The invention relates to the technical field of hops, and is a kind of supercritical CO 2 The method for extracting xanthohumol in hop slag and the preparation of xanthohumol product. Background technique [0002] Xanthonumol (Xanthonumol) is a functional substance unique to hops (Humulus lupulus L.). Xanthohumol is a flavonoid compound containing isoprenyl group (structure such as figure 1 Shown), hops are the only source of natural isoprenyl flavonoids discovered so far. The content of xanthohumol in hops is only 0.1% to 1.0%. [0003] Xanthohumol was first discovered in hops in 1913. Research on its molecular structure began in 1950. At that time, researchers did not pay attention to its health effects. It was not until 1990 that the effect of this substance was obtained. know. Studies have found that the xanthohumol in hops can prevent the enzymes that cause cancer cells from working, and can help the body eliminate other carcinogens, especially in the...
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