CN103622134B - Be that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses - Google Patents

Be that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses Download PDF

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CN103622134B
CN103622134B CN201310567410.XA CN201310567410A CN103622134B CN 103622134 B CN103622134 B CN 103622134B CN 201310567410 A CN201310567410 A CN 201310567410A CN 103622134 B CN103622134 B CN 103622134B
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molasses
extraction
raw material
oxidant
food preservative
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CN103622134A (en
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孟赫诚
陈明舜
于淑娟
扶雄
管永光
唐强
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Guangdong Huazhi Sugar Health Food Co.,Ltd.
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South China University of Technology SCUT
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3472—Compounds of undetermined constitution obtained from animals or plants

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Botany (AREA)
  • Nutrition Science (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses with molasses is that raw material preparation has anti-oxidant and method that is biocidal property food preservative.Molasses raw material and entrainer are first carried out ultrasonic pretreatment by the method, and ultrasonic power is 100 ~ 500W, and temperature is 10 DEG C ~ 70 DEG C, and the time is 1min ~ 30min; Entrainer is nontoxic volatile organic solvent; Entrainer consumption is 30% ~ 90% of molasses raw material volume; Pretreated material loads in supercritical fluid extraction equipment; Supercritical CO 2the extraction kettle pressure of fluid extraction is 5MPa ~ 50Mpa, and Rectification column pressure is 1MPa ~ 15Mpa, and extraction time is 20min ~ 120min; Extraction kettle temperature is 20 DEG C ~ 90 DEG C, and rectifying column temperature is 10 DEG C ~ 150 DEG C; The food preservative yield that the present invention obtains is high, quality better, belongs to natural extract, no solvent residue, edible safety, gives off a strong fragrance pure, have anti-oxidant and antibacterial effect.

Description

Be that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses
Technical field
The present invention relates to molasses, particularly a kind of is that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses, belongs to the green manufacture field of food.
Background technology
Natural and anticorrisive agent are the typical additives in food, health products, although its consumption is less, its effect and added value are very considerable.Molasses are accessory substances of sugar industry, and its physical behavior is a kind of thickness, dark brown, the dynamic body of paste in semi-fluid.Molasses components is complicated, except containing except 30% ~ 50% sucrose and reduced sugar, also containing compositions such as colloid, inorganic ash content, flavones, Polyphenols and large molecule aroma substances.Shi Chantang big country of China, sugar material is planted in agricultural economy and occupies critical role, is only second to grain, oil plant, cotton.The domestic molasses annual production about 4,800,000 tons for utilizing.Fermentation process is generally adopted to prepare the products such as alcohol, yeast, lactic acid, citric acid, lysine at present.Produce above-mentioned fermented product and only make use of sugar in blackstrap, other organic substance such as phenol sulfonate, amino acid, protein and aromatic substance are all stayed in useless mash, make COD and the BOD value of the downstream product waste water of molasses fermented preparation high, one of five large pollution sources becoming China.As extracted high-quality natural and food preservative from molasses, not only edible safety and also the sense of taste fine, can greatly improve molasses added value.
The method that tradition extracts natural products is organic solvent extractionprocess, though the method is relatively easy, solvent residual amount is large, in order to make product not containing toxic component, causing subsequent treatment process complicated, but also bringing emission pollution problem.Chinese invention patent CN102499459A discloses a kind of natural plant essential oils and preparation method thereof and the application in cigarette, it is dry after plant is cleaned, Plant Powder is obtained through pulverizing, by Plant Powder in sodium-chloride water solution in 80 DEG C ?distill at 100 DEG C 8 little Shi ?12 hours, collect volatile matter and obtain faint yellow essential oil, obtain plants essential oil through post processing.It is the method that essential oil prepared by raw material that Chinese invention patent CN101455326 discloses with molasses, adopt hot acid method's acidolysis, add phosphoric acid, use milk of lime adjust pH, flocculation, centrifugal, add amino acid, adjust pH carries out carbonyl ammonia react again, extracts lower boiling volatile fragrant components, concentrates extract, obtains described essential oil.Though above-mentioned two kinds of preparation methods can prepare natural products, technique is comparatively complicated, and need add a large amount of solvent.In addition, above-mentioned two kinds of methods all adopt long-time high-temperature process, and preparation time is long, not only the amount of disappearing, and easily destroy the active ingredients such as anti-oxidant in food preservative and biocidal property.
Summary of the invention
The object of the present invention is to provide that a kind of product yield is high, preparation time is short, extraction efficiency is high, and the profit of environmental protection is that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses.
Supercritical CO 2abstraction technique is ripe in some chemical sector applications, but is used in due to its complicated components in molasses extraction, and extraction efficiency is low, and power consumption and the entrainer consumption of process are high.The present invention adopts ultrasonic wave added supercritical CO 2abstraction technique, utilizes ultrasonic cavitation to change form and the volume structure of molasses in extraction equipment, makes volatile component be easy to be separated from stickum, thus strengthening leaching process.Ultrasonic wave added supercritical CO 2extract by regulating ultrasonic power, temperature, the temperature and pressure of supercritical fluids system, makes fluid be in supercriticality, greatly increases some organic solubility.Ultrasonic wave added supercritical CO 2extraction has high, the superior product quality of extraction yield, saves energy consumption, the features such as protection of the environment, is suitable for being separated the material containing heat-sensitive component and physiological activator.
The present invention adopts ultrasonic wave added supercritical CO 2fluid extraction technology, by changing extraction conditions, from molasses raw material, extraction obtains anti-oxidant and biocidal property material.Feature of the present invention carries high product yield, shortening preparation time, improves extraction efficiency, strengthen edible safety, avoid environmental pollution.The inventive method technological process is short, method is simple; With CO 2for solvent, both free from environmental pollution, the pure natural characteristic of product can be kept again, and CO 2can be recycled.
Object of the present invention is achieved through the following technical solutions:
Be that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses, comprise the steps:
(1) first molasses raw material and entrainer are carried out ultrasonic pretreatment, the ultrasonic power of described ultrasonic pretreatment is 100 ~ 500W, and temperature is 10 DEG C ~ 70 DEG C, and the time is 1min ~ 30min; Described entrainer is nontoxic volatile organic solvent; Entrainer consumption is 30% ~ 90% of molasses raw material volume;
(2) pretreated material loads in the extraction kettle of supercritical fluid extraction equipment; Supercritical CO is set 2the extraction kettle pressure of fluid extraction is 5MPa ~ 50Mpa, and Rectification column pressure is 1MPa ~ 15Mpa, and extraction time is 20min ~ 120min; Extraction kettle temperature is 20 DEG C ~ 90 DEG C, and rectifying column temperature is 10 DEG C ~ 150 DEG C;
(3), after having extracted, with receiver collection material from rectifying column, the material of reception is concentrated, obtain can be anti-oxidant and antibacterial food preservative.
For realizing the object of the invention further, described molasses raw material is the thick liquid by-product after sugarcane, beet, soybean or starch isolation sugar.
Described entrainer is ethanol and/or ethyl acetate.Or described entrainer is benzinum.
It is through freeze concentration or reduced pressure concentration by the material collected in rectifying column that the material of step (3) concentrates.
Ultrasonic wave added supercritical CO of the present invention 2fluid extraction process is: molasses in extraction kettle by CO 2fluid extraction; After having extracted, be extracted component and CO 2fluid enters rectifying column, and carries out CO in rectifying column 2fluid is separated thus obtains having anti-oxidant and biocidal property food preservative molasses from rectifying column.
Compared with prior art, the present invention has the following advantages:
(1) ultrasonic wave added supercritical CO is adopted 2fluid extraction extracts anti-oxidant in molasses and biocidal property food preservative, and its preparation time is no more than 120min, than Conventional espresso method 8 ~ 12 little time preparation time shorten 3 ~ 5 times;
(2) ultrasonic wave added supercritical CO 2fluid extraction temperature is relatively low, can not cause anti-oxidant being destroyed with biocidal property composition or generation poisonous and harmful substance, and energy-saving and cost-reducing;
(3) ultrasonic wave added supercritical CO 2in fluid extraction molasses, anti-oxidant and biocidal property material effectively removes heavy metal in molasses and colloid, simplifies isolation and purification process;
(4) owing to not adding other chemical reagent in preparation process, avoid product poisonous and harmful substance and remain the disposal of pollutants with separation and purification.
Detailed description of the invention
Be described further the present invention below in conjunction with embodiment, it should be noted that, embodiment does not form the restriction to application claims protection domain.
Embodiment 1:
Select Huaan, Nantong supercritical extracting equipment Co., Ltd produce HA120 ?50 ?02 type supercritical fluid extraction instrument as supercritical CO 2fluid extraction device, the extraction kettle volume of this device is 2L; High-pressure pump maximum pressure is 60Mpa; Extraction kettle, rectifying column heater maximum heating temperature are 90 DEG C.
Get the cane molasses 1L that Guangdong DongTang Group provides, load in ultrosonic extractor, the ethanol adding cane molasses quality 50%, as entrainer, fully shakes up, and makes mixed solution.This mixed solution is carried out super ultrasonic wave extraction, it is as follows that Ultrasonic Conditions is set: (1) ultrasonic power: 300W; (2) temperature: 40 DEG C; (3) time: 5min.This ultrasonic complete mixed solution is carried out supercritical CO 2fluid extraction, arranges extraction conditions as follows: (1) extraction kettle pressure: 25Mpa, Rectification column pressure: 6Mpa; (2) extraction time: 60min; (3) extraction kettle temperature: 40 DEG C, rectifying column temperature: 40 DEG C.Supercritical CO 2after fluid extraction completes, in rectifying column, obtain liquid material, concentrate through rotary evaporation, anti-oxidant and biocidal property food preservative must be had.
After testing, the anti-oxidant value of gained food preservative is 5500ORAC unit; Its freeze drying is dissolved in physiological saline, and through K ?B paper disk method measure inhibition zone, find that it is all greater than 15mm to Escherichia coli, staphylococcus aureus, Listeria monocytogenes and salmonella inhibition zone.The anticorrisive agent recovery rate that molasses extract is 82%.
Embodiment 2:
Select Liaoning Histar Bio-tech Co., Ltd. produce SFE240 ?40 ?30 type supercritical fluid extraction instruments as supercritical CO 2fluid extraction device, the extraction kettle volume of this device is 20L; High-pressure pump maximum pressure is 60Mpa; Extraction kettle, rectifying column heater maximum heating temperature are 90 DEG C.
The beet molasses 10L that Qu Botian sugar industry Co., Ltd provides, load in ultrosonic extractor, the ethyl acetate adding beet molasses quality 30%, as entrainer, fully shakes up, and makes mixed solution.This mixed solution is carried out super ultrasonic wave extraction, it is as follows that Ultrasonic Conditions is set: (1) ultrasonic power: 100W; (2) temperature: 20 DEG C; (3) time: 20min.This ultrasonic complete mixed solution is carried out supercritical CO 2fluid extraction, arranges extraction conditions as follows: (1) extraction kettle pressure: 20Mpa, Rectification column pressure: 5Mpa; (2) extraction time: 30min; (3) extraction kettle temperature: 70 DEG C, rectifying column temperature: 70 DEG C.Supercritical CO 2after fluid extraction completes, in rectifying column, obtain liquid material, concentrate through rotary evaporation, anti-oxidant and biocidal property food preservative must be had.
After testing, the anti-oxidant value of gained food preservative is 2300ORAC unit; Its freeze drying is dissolved in physiological saline, and through K ?B paper disk method measure inhibition zone, find it to Escherichia coli, staphylococcus aureus, Listeria monocytogenes and salmonella inhibition zone at about 12mm.The anticorrisive agent recovery rate that molasses extract is 75%.
Embodiment 3:
Select Kaiyuan chemical machinery Group Co., Ltd produce SFE430 ?40 ?150 type supercritical fluid extraction instruments as supercritical CO 2fluid extraction device, the extraction kettle volume of this device is 35L; High-pressure pump maximum pressure is 50Mpa; Extraction kettle, rectifying column maximum heating temperature are 85 DEG C.
Get the cane molasses 10L that Suixi County, Guangdong Nan Jian sugar industry Co., Ltd provides, load in ultrosonic extractor, the benzinum adding cane molasses quality 50%, as entrainer, fully shakes up, and makes mixed solution.This mixed solution is carried out super ultrasonic wave extraction, it is as follows that Ultrasonic Conditions is set: (1) ultrasonic power: 500W; (2) temperature: 50 DEG C; (3) time: 3min.This ultrasonic complete mixed solution is carried out supercritical CO 2fluid extraction, arranges extraction conditions as follows: (1) extraction kettle pressure: 15Mpa, Rectification column pressure: 4Mpa; (2) extraction time: 120min; (3) extraction kettle temperature: 30 DEG C, rectifying column temperature: 30 DEG C.Supercritical CO 2after fluid extraction completes, in rectifying column, obtain liquid material, concentrate through rotary evaporation, anti-oxidant and biocidal property food preservative must be had.
After testing, the anti-oxidant value of gained food preservative is 1100ORAC unit; Its freeze drying is dissolved in physiological saline, and through K ?B paper disk method measure inhibition zone, find that it is about 10mm to Escherichia coli, staphylococcus aureus, Listeria monocytogenes and salmonella inhibition zone size.The anticorrisive agent recovery rate that molasses extract is 70%.
Embodiment 4:
Select Nantong Huaxing Petroleum Instrument Co., Ltd. produce SFE420 ?50 ?200 type supercritical fluid extraction instruments as supercritical CO 2fluid extraction device, the extraction kettle volume of this device is 50L; High-pressure pump maximum pressure is 50Mpa; Extraction kettle, rectifying column heater maximum heating temperature are 90 DEG C.
Get the cane molasses 15L that Nanning candy paper Co., Ltd., Factory provides, load in ultrosonic extractor, add cane molasses mass fraction 70% 1:1 by volume prepare Yi Chun ?ethyl acetate as entrainer, due to ethanol and ethyl acetate can by arbitrary volume than miscible as entrainer, and entrainer add the polarity that can improve fluid, according to the similar principle that mixes, the polarity improving fluid can obtain the extraction product of relative high polarity in extraction process, therefore selects the second alcohol ?ethyl acetate of volume ratio 1:1 as entrainer.After adding entrainer, fully shake up, make mixed solution.This mixed solution is carried out super ultrasonic wave extraction, it is as follows that Ultrasonic Conditions is set: (1) ultrasonic power: 400W; (2) temperature: 45 DEG C; (3) time: 10min.This ultrasonic complete mixed solution is carried out supercritical CO 2fluid extraction, arranges extraction conditions as follows: (1) extraction kettle pressure: 35Mpa, Rectification column pressure: 6Mpa; (2) extraction time: 100min; (3) extraction kettle temperature: 45 DEG C, rectifying column temperature: 45 DEG C.Supercritical CO 2after fluid extraction completes, in rectifying column, obtain liquid material, concentrate through rotary evaporation, anti-oxidant and biocidal property food preservative must be had.
After testing, the anti-oxidant value of gained food preservative is 7800ORAC unit; Its freeze drying is dissolved in physiological saline, and through K ?B paper disk method measure inhibition zone, find it to Escherichia coli, staphylococcus aureus, Listeria monocytogenes and salmonella inhibition zone size at about 18mm.The anticorrisive agent recovery rate that molasses extract is 90%.
As can be seen from the above embodiments, through the ultrasonic assistant supercritical CO of different condition 2fluid extraction process molasses material, can prepare and can meet the industrial anti-oxidant and biocidal property food preservative product of having, expand the scope of application of molasses.Compared with Conventional espresso method treatment technology, adopt supercritical CO 2fluid extraction extracts anti-oxidant in molasses and biocidal property food preservative, and its preparation time is no more than 120min, than Conventional espresso method 8 ~ 12 little time preparation time shorten 3 ~ 5 times.Ultrasonic assistant supercritical CO 2fluid extraction temperature, at 30 DEG C ~ 70 DEG C, can not cause anti-oxidant destroyed with biocidal property composition, economize energy simultaneously.Ultrasonic assistant supercritical CO 2fluid extraction extracts anti-oxidant in molasses and biocidal property food preservative and effectively removes heavy metal in molasses and colloid.Food preservative main component of its anti-oxidant and biocidal property performance by GC ?MS detect, for palmitic acid and 2,2' ?Ya Jia Ji bis-?(4 ?Jia Ji ?6 ?tert-butyl phenol), its anti-oxidant value can up to 7800ORAC unit, higher than the 5200ORAC unit of blueberry, it can reach 18mm to Escherichia coli, staphylococcus aureus, Listeria monocytogenes and salmonella inhibition zone, belongs to high quick biocidal property.Owing to not adding other chemical reagent in preparation process, avoid product poisonous and harmful substance and remain the disposal of pollutants with separation and purification.

Claims (3)

1. be that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses, it is characterized in that comprising the steps:
(1) first molasses raw material and entrainer are carried out ultrasonic pretreatment, the ultrasonic power of described ultrasonic pretreatment is 100 ~ 500W, and temperature is 10 DEG C ~ 70 DEG C, and the time is 1min ~ 30min; Described entrainer is nontoxic volatile organic solvent; Entrainer consumption is 30% ~ 90% of molasses raw material volume; Described molasses raw material is the thick liquid by-product after sugarcane, beet, soybean or starch isolation sugar;
(2) pretreated material loads in the extraction kettle of supercritical fluid extraction equipment; Supercritical CO is set 2the extraction kettle pressure of fluid extraction is 5MPa ~ 50Mpa, and Rectification column pressure is 1MPa ~ 15Mpa, and extraction time is 20min ~ 120min; Extraction kettle temperature is 20 DEG C ~ 90 DEG C, and rectifying column temperature is 10 DEG C ~ 150 DEG C;
(3), after rectifying completes, with receiver collection material from rectifying column, the material of reception is concentrated, obtain can be anti-oxidant and antibacterial food preservative.
2. according to claim 1 is that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses, it is characterized in that: described entrainer is ethanol and/or ethyl acetate.
3. according to claim 1 is that raw material preparation has anti-oxidant and method that is biocidal property food preservative with molasses, it is characterized in that: it is through freeze concentration or reduced pressure concentration by the material collected in rectifying column that the material of step (3) concentrates.
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CN104738311B (en) * 2014-12-26 2018-02-02 东莞市银华生物科技有限公司 A kind of fish slurry fermented bean dregs and its production method and application
CN107981044A (en) * 2017-12-13 2018-05-04 临沧宏胜生物科技开发有限公司 Feed/food additives made of one kind molasses and/or blackstrap
CN109156793A (en) * 2018-08-14 2019-01-08 华南理工大学 A kind of flavor dressing agent and preparation method thereof

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