CN114831305A - Method for preparing hop by modification - Google Patents

Method for preparing hop by modification Download PDF

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Publication number
CN114831305A
CN114831305A CN202210414280.5A CN202210414280A CN114831305A CN 114831305 A CN114831305 A CN 114831305A CN 202210414280 A CN202210414280 A CN 202210414280A CN 114831305 A CN114831305 A CN 114831305A
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China
Prior art keywords
cannabidiol
hop
hops
mixture
mixture obtained
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Pending
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CN202210414280.5A
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Chinese (zh)
Inventor
苏云鹏
杨冠英
张筱岚
赵媛
张颖
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Dali University
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Dali University
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Priority to CN202210414280.5A priority Critical patent/CN114831305A/en
Publication of CN114831305A publication Critical patent/CN114831305A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Mycology (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Botany (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention discloses a method for preparing modified hops, which adopts a chelation method, and comprises the steps of ultrasonically dissolving dried hop powder, cellulase and ethanol, keeping the temperature at 50-60 ℃ for 1-4h, ultrasonically dissolving cannabidiol, a surfactant and pure water, adding the dissolved solution into the solution, ultrasonically mixing the solution at normal pressure in an ultrasonic mixer, and concentrating and drying the solution under reduced pressure to obtain hops containing active cannabidiol; the method effectively improves the active factors of the hops, introduces the cannabidiol modified substances, ensures that the hops after modification have the effects of antibiosis, antiphlogosis, pressure resistance and the like, has better development prospect, and is easy to realize industrial production.

Description

Method for preparing hop by modification
Technical Field
The invention belongs to the field of food and health care products, and particularly relates to a hop modification preparation method containing active cannabidiol.
Background
The alcohol blossom is known as the spirit of beer and becomes one of the indispensable raw materials for brewing beer. Hops can not only serve as a natural preservative in beer, but also impart unique bitterness and aroma characteristics to beer. The quality or modification of hops directly affects the quality of beer, wherein the resinous components, volatile oils and polyphenols affect the taste and flavor of the beer. The hop has strong medicinal value: the alpha-acid and the beta-acid in the hop have good antibacterial action; the oxidation resistance is realized, and alpha-acid and hydrogenation products thereof, beta-acid and polyphenol substances in the hop have the oxidation resistance; the resin component in flos Lupuli has antitumor effect, and can inhibit human gastric adenocarcinoma cell CRL-1793 and mastadenoma cell-A-427; has the protective effect on the cardiovascular system, and quercetin, rutin and the like in the hops can prevent blood platelets from aggregating, thereby playing the roles of anticoagulation and blood vessel protection. Therefore, the modification of hops is a major research and development direction in this field.
Cannabidiol has the effects of analgesia, intraocular pressure reduction, antibiosis, anti-inflammation, thrombus resistance and the like, and has strong potential application value in the fields of medicine, food and the like.
According to the invention, cannabidiol is added into the hops, so that the content of phenols in the hops is effectively increased, and the hop is an ideal addition mode, so that more modification space is provided for beer brewing.
The same literature disclosures as the technical scheme of the invention are not found at present.
Disclosure of Invention
The invention aims to provide a preparation method for hop modification, which enriches the functionalization of hops in beer, cannabidiol is an important beneficial component, the added value of materials is improved through deep processing, and the preparation method has obvious significance for national economic construction, but cannabidiol is not easy to be comprehensively utilized, so how to comprehensively utilize cannabidiol and improve the application performance of cannabidiol is one of important research points; the invention prepares the hop containing the active cannabidiol by modifying the hop, and effectively combines the cannabidiol and the hop.
The preparation method of the hop containing the active cannabidiol comprises the following steps:
(1) ultrasonically dispersing dried hop powder and cellulase in ethanol, and keeping the water bath at the temperature of 50-60 ℃ for 1-4 h;
the mass ratio of the hop dry powder to the ethanol is 1:5-1:20, and the addition amount of the cellulase is 0.5% -5% of the mass of the hop dry powder.
The cellulase is one or more of exo-beta-glucanase, endo-beta-glucanase, beta-glucosidase and xylanase;
(2) mixing cannabidiol, surfactant and pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersed liquid into the mixture obtained in the step (1), stirring to uniformly mix the dispersed liquid, and adjusting the pH value of the mixture to 7-8;
the surfactant is one or more of polyethylene glycol, sodium dodecyl benzene sulfonate, polysorbate-80 and ethyl acetate, the addition amount of the surfactant is 0.05-1% of the mass of the dried hop powder, and the addition amount of the cannabidiol is 0.1-1% of the mass of the dried hop powder.
The pH regulator is one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium carbonate and potassium bicarbonate, and the quality of the pure water is equal to that of the dried hop powder in the step 1.
(3) Ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer at normal pressure for 30-60 min;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, controlling the temperature at 40-75 ℃, and concentrating and drying under reduced pressure to obtain the hop containing the active cannabidiol.
Using a chromatographic column: InertSustain C18, isocratic elution with methanol-water (85: 15) as the mobile phase. Under the chromatographic condition, a CBD reference substance and a hop sample containing active cannabidiol are respectively injected and analyzed.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method is simple, low in cost and mild in reaction condition;
(2) the cannabidiol is added in a milder reaction mode without damaging the active ingredients of the hop material;
(3) the raw materials adopted by the invention are environment-friendly, the process is simple, and the industrial production is easy to realize.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited to the above-mentioned descriptions.
Example 1:
(1) ultrasonically dispersing 100g of hop dry powder and 0.5g of cellulase in 500g of ethanol, and then keeping the constant temperature of a water bath at 50 ℃ for 3 hours;
(2) mixing 0.1g of cannabidiol, 0.05g of polyethylene glycol and 100g of pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersed liquid into the mixture obtained in the step (1), stirring to uniformly mix the dispersed liquid and the mixture, and adjusting the pH value of the mixture to 7 by adopting sodium carbonate;
(3) ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer at normal pressure for 30 min;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, controlling the temperature at 60 ℃, and performing reduced pressure concentration and drying to obtain the hop containing the active cannabidiol.
Hops of active cannabidiol prepared in this example were purified using a chromatographic column: InertSustain C18, and performing isocratic elution by using methanol-water (volume ratio is 85: 15) as a mobile phase; under the chromatographic condition, a CBD reference substance and a hop sample containing active cannabidiol are respectively injected and analyzed. The result shows that the hop of the active cannabidiol contains 350mg/kg of the active cannabidiol.
Example 2:
(1) dispersing 200g of hop dry powder and 2g of cellulase in 500g of ethanol by ultrasonic, and keeping the water bath at the temperature of 60 ℃ for 2 hours;
(2) mixing 2g of cannabidiol, 0.16g of polysorbate-80 and 200g of pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersion liquid into the mixture obtained in the step (1), stirring to uniformly mix the mixture, and adjusting the pH value of the mixture to 8 by using sodium bicarbonate;
(3) ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer at normal pressure for 60 min;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, controlling the temperature at 50 ℃, and concentrating and drying under reduced pressure to obtain the hop containing the active cannabidiol.
Hops of active cannabidiol prepared in this example were purified using a chromatographic column: InertSustain C18, and performing isocratic elution by using methanol-water (85: 15) as a mobile phase; under the chromatographic condition, the CBD reference substance and the hop sample containing the active cannabidiol are respectively injected and analyzed, and the result shows that the hop containing the active cannabidiol has the active cannabidiol content of 4200 mg/kg.
Example 3:
(1) dispersing 300g of hop dry powder and 6g of cellulase in 500g of ethanol by ultrasonic, and then keeping the constant temperature of 55 ℃ water bath for 2 h;
(2) mixing 1.5g of cannabidiol, 3g of sodium dodecyl benzene sulfonate and 300g of pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersed liquid into the mixture obtained in the step (1), stirring to uniformly mix the dispersed liquid and the mixture, and adjusting the pH value of the mixture to 7 by using sodium hydroxide;
(3) ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer at normal pressure for 40 min;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, controlling the temperature at 60 ℃, and carrying out reduced pressure concentration and drying to obtain the hop containing the active cannabidiol.
Hops of active cannabidiol prepared in this example were purified using a chromatographic column: InertSustain C18, isocratic elution with methanol-water (85: 15) as the mobile phase. Under the chromatographic condition, a CBD reference substance and a hop sample containing the active cannabidiol are taken for sample injection analysis respectively, and the result shows that the hop containing the active cannabidiol has the active cannabidiol content of 1800 mg/kg.
Example 4:
(1) dispersing 400g of hop dry powder and 10g of cellulase in 500g of ethanol by ultrasonic, and keeping the constant temperature of 55 ℃ water bath for 3 h;
(2) mixing 2g of cannabidiol, 0.05g of sodium dodecyl benzene sulfonate and 400g of pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersed liquid into the mixture obtained in the step (1), stirring to uniformly mix the dispersed liquid and the mixture, and adjusting the pH value of the mixture to 7 by using sodium carbonate;
(3) ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer for 50min at normal pressure;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, controlling the temperature at 40 ℃, and concentrating and drying under reduced pressure to obtain the hop containing the active cannabidiol.
Hops of active cannabidiol prepared in this example were purified using a chromatographic column: InertSustain C18, and performing isocratic elution by using methanol-water (85: 15) as a mobile phase; under the chromatographic condition, a CBD reference substance and a hop sample containing active cannabidiol are respectively injected and analyzed. The result shows that the hop of the active cannabidiol contains 1800mg/kg of the active cannabidiol.

Claims (5)

1. A method for modifying and preparing hop is characterized by comprising the following specific steps:
(1) ultrasonically dispersing dried hop powder and cellulase in ethanol, and keeping the water bath at the temperature of 50-60 ℃ for 1-4 h;
(2) mixing cannabidiol, surfactant and pure water, performing ultrasonic treatment until the mixture is uniformly dispersed, dropwise adding the dispersed liquid into the mixture obtained in the step (1), stirring to uniformly mix the dispersed liquid, and adjusting the pH value of the mixture to 7-8;
(3) ultrasonically mixing the mixture obtained in the step (2) in an ultrasonic mixer at normal pressure for 30-60 min;
(4) and (4) transferring the mixture obtained in the step (3) to a multi-effect external circulation evaporator, and performing reduced pressure concentration and drying to obtain the hop containing the active cannabidiol.
2. The method for the modified preparation of hops according to claim 1, characterized in that: the addition amount of the cellulase is 0.5-5% of the mass of the dried hop powder.
3. The method for the modified preparation of hops according to claim 1, characterized in that: the surfactant is one or more of polyethylene glycol, sodium dodecyl benzene sulfonate, polysorbate-80 and ethyl acetate, the addition amount of the surfactant is 0.05-1% of the mass of the dried hop powder, and the addition amount of the cannabidiol is 0.1-1% of the mass of the dried hop powder.
4. The method for the modified preparation of hops according to claim 1, characterized in that: the pH regulator is one or more of sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium carbonate and potassium bicarbonate.
5. The method for the modified preparation of hops according to claim 1, characterized in that: the temperature of the multi-effect external circulation evaporator is 40-75 ℃.
CN202210414280.5A 2022-04-20 2022-04-20 Method for preparing hop by modification Pending CN114831305A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070254063A1 (en) * 2006-04-07 2007-11-01 Chemisch En Biochemisch Onderzoekscentrum (Cbok) Use of hop polyphenols in beer
CN112680301A (en) * 2021-01-19 2021-04-20 哈尔滨宝邦生物科技发展有限公司 Beer making process with CBD
CN113234552A (en) * 2021-04-29 2021-08-10 浙江大学 Hop polysaccharide nano particle and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070254063A1 (en) * 2006-04-07 2007-11-01 Chemisch En Biochemisch Onderzoekscentrum (Cbok) Use of hop polyphenols in beer
CN112680301A (en) * 2021-01-19 2021-04-20 哈尔滨宝邦生物科技发展有限公司 Beer making process with CBD
CN113234552A (en) * 2021-04-29 2021-08-10 浙江大学 Hop polysaccharide nano particle and preparation method and application thereof

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