CN107510057A - A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere - Google Patents

A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere Download PDF

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Publication number
CN107510057A
CN107510057A CN201710934867.8A CN201710934867A CN107510057A CN 107510057 A CN107510057 A CN 107510057A CN 201710934867 A CN201710934867 A CN 201710934867A CN 107510057 A CN107510057 A CN 107510057A
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fat
fish oil
soluble tea
tea polyphenol
mackerel
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CN201710934867.8A
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庞婉青
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Wuxi Sheng Ya Biological Science And Technology Co Ltd Foshan Branch
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Wuxi Sheng Ya Biological Science And Technology Co Ltd Foshan Branch
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Publication of CN107510057A publication Critical patent/CN107510057A/en
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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
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • 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
    • A23L33/115Fatty acids or derivatives thereof; Fats or oils
    • A23L33/12Fatty acids or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • 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

Abstract

The invention provides the preparation method of a kind of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprise the following steps:Mackerel fish head is taken to extract fish oil;By fat-soluble tea polyphenol dissolving wherein, miscella is obtained;PLA and miscella are dissolved in chloroform and acetone respectively, it is uniformly ultrasonic after blending to obtain dispersed phase;Sorbitan oleate, polyoxyethylene sorbitol acid anhydride monopalmitate and polyvinyl alcohol are added to stirring and dissolving in deionized water and obtain continuous phase;It is added to scattered in holder, dispersed phase is pressed into continuous phase by SPG microporous barriers, obtains monodispersed O/W types emulsion;It is transferred in thermostat and stirs, is finally solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;It is washed with deionized, is produced after freeze-drying.Mackerel fish oil and fat-soluble tea polyphenol complex microsphere prepared by this method carry mackerel oil mass and Tea Polyphenols amount is all higher, and inoxidizability is fine, while has good releasing effect, can be absorbed well by enteron aisle.

Description

A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere
Technical field
The present invention relates to the preparation method of a kind of mackerel fish oil and fat-soluble tea polyphenol complex microsphere.
Background technology
Mackerel, belong to Perciformes, mackerel section, chub mackerel category.Local name oil cylinder fish, blue and white fish etc., for economic fish at the middle and upper levels, mainly Be distributed in Western North Pacific Ocean, be distributed in each marine site in China, the East Sea and the Huanghai Sea are the abundantest, be distributed in the East Sea and The mackerel of the Huanghai Sea is divided into two kinds of common Japanese mackere and Australia chub mackerel, and the yield of East China Sea region mackerel is 20 × 10 in recent years4Ton or so, Huanghai Sea area The yield of mackerel is in (11~12) × 104Ton, it is one of important economic fish in China.At present, the utilization of mackerel is mainly in chub mackerel The processing of fish product, but many accessory substances such as internal organ, fish head, fish-bone, fish tail can be produced during processing, account for it The 30~40% of body weight, these accessory substances contain the active ingredients such as abundant fat, protein, amino acid and trace element, such as Fruit, which is not used, can cause to waste.The good method that fish oil is exactly a by-product utilized, the opposing party are extracted from mackerel fish head Face, at present, fish oil all use microencapsulation, and microballoon is mainly used in the load of medicine, and fish oil are carried in microballoon, energy More preferably digested and assimilated by enteron aisle, preferably protect unrighted acid to be utilized.
The content of the invention
Technical problems to be solved:It is an object of the invention to provide a kind of mackerel fish oil and fat-soluble tea polyphenol complex microsphere Preparation method, the particle size of prepared mackerel fish oil and fat-soluble tea polyphenol complex microsphere 21.43-21.53 μm it Between, carry mackerel oil mass and Tea Polyphenols amount is all higher, inoxidizability is fine, while has good releasing effect, can be by enteron aisle very Good absorbs.
Technical scheme:A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil after crushing;
S2:By 0.5-0.8g fat-soluble tea polyphenols stirring and dissolving in 5-10g mackerel fish oil, miscella is obtained;
S3:4-8g PLAs and miscella are dissolved in 50-80mL chloroforms and 100-150mL acetone respectively, and are sufficiently stirred, altogether It is uniformly ultrasonic after mixed to obtain dispersed phase;
S4:0.8-1g sorbitan oleates, 0.2-0.5g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.5-1g are gathered Vinyl alcohol is added in 500-700mL deionized waters, and heating water bath is sufficiently stirred to 80-95 DEG C and dissolves to obtain continuous phase;
S5:It is added to scattered in holder, under impressed pressure 0.045-0.050MPa effects, will be divided by SPG microporous barriers In dephasing press-in continuous phase, monodispersed O/W types emulsion is obtained;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, 6-8 hours are stirred with rotating speed 520-570r/min, with chloroform With the volatilization of acetone, mackerel fish oil and fat-soluble tea polyphenol complex microsphere are finally solidified into;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged into 30-35 under rotating speed 7500-8000r/min Minute, it is washed with deionized 3 times, is produced after freeze-drying.
Further, supercritical extract condition is that extraction temperature is 45-60 DEG C in S1, extracting pressure 35-45MPa, during extraction Between be 2-3 hours.
It is further preferred that rotating speed is 550r/min in S6, mixing time is 7 hours.
It is further preferred that rotating speed is 7800r/min in S7, centrifugation time is 33 minutes.
Beneficial effect:The particle size of mackerel fish oil and fat-soluble tea polyphenol complex microsphere prepared by the present invention is in 21.43- Between 21.53 μm, load mackerel oil mass is higher, reaches as high as 64.95%, and it is up to 17.44% to carry Tea Polyphenols amount, clear for DPPH Except rate is up to 59.98%, inoxidizability is fine, while envelop rate also can reach 19.86%, has good releasing effect, It can be absorbed well by enteron aisle.
Embodiment
Embodiment 1
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil, extraction temperature 45 after crushing DEG C, extracting pressure 35MPa, extraction time is 2 hours;
S2:By 0.5g fat-soluble tea polyphenols stirring and dissolving in 5g mackerel fish oil, miscella is obtained;
S3:4g PLAs and miscella are dissolved in 50mL chloroforms and 100mL acetone respectively, and are sufficiently stirred, after blending uniformly It is ultrasonic to obtain dispersed phase;
S4:0.8g sorbitan oleates, 0.2g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.5g polyvinyl alcohol are added Enter into 500mL deionized waters, heating water bath is sufficiently stirred to 80 DEG C and dissolves to obtain continuous phase;
S5:Scattered it will be added in holder, under impressed pressure 0.045MPa effects, by SPG microporous barriers by dispersed phase pressure Enter in continuous phase, obtain monodispersed O/W types emulsion;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, stirred 6 hours with rotating speed 520r/min, with chloroform and acetone Volatilization, be finally solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged 30 minutes under rotating speed 7500r/min, spent Ion water washing 3 times, is produced after freeze-drying.
Embodiment 2
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil, extraction temperature 50 after crushing DEG C, extracting pressure 38MPa, extraction time is 2 hours;
S2:By 0.6g fat-soluble tea polyphenols stirring and dissolving in 6g mackerel fish oil, miscella is obtained;
S3:5g PLAs and miscella are dissolved in 60mL chloroforms and 110mL acetone respectively, and are sufficiently stirred, after blending uniformly It is ultrasonic to obtain dispersed phase;
S4:0.9g sorbitan oleates, 0.3g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.6g polyvinyl alcohol are added Enter into 550mL deionized waters, heating water bath is sufficiently stirred to 85 DEG C and dissolves to obtain continuous phase;
S5:Scattered it will be added in holder, under impressed pressure 0.046MPa effects, by SPG microporous barriers by dispersed phase pressure Enter in continuous phase, obtain monodispersed O/W types emulsion;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, stirred 6.5 hours with rotating speed 540r/min, with chloroform and third The volatilization of ketone, finally it is solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged 32 minutes under rotating speed 7600r/min, spent Ion water washing 3 times, is produced after freeze-drying.
Embodiment 3
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil, extraction temperature 55 after crushing DEG C, extracting pressure 40MPa, extraction time is 3 hours;
S2:By 0.7g fat-soluble tea polyphenols stirring and dissolving in 9g mackerel fish oil, miscella is obtained;
S3:7g PLAs and miscella are dissolved in 70mL chloroforms and 140mL acetone respectively, and are sufficiently stirred, after blending uniformly It is ultrasonic to obtain dispersed phase;
S4:0.9g sorbitan oleates, 0.4g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.8g polyvinyl alcohol are added Enter into 600mL deionized waters, heating water bath is sufficiently stirred to 90 DEG C and dissolves to obtain continuous phase;
S5:Scattered it will be added in holder, under impressed pressure 0.049MPa effects, by SPG microporous barriers by dispersed phase pressure Enter in continuous phase, obtain monodispersed O/W types emulsion;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, stirred 7 hours with rotating speed 550r/min, with chloroform and acetone Volatilization, be finally solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged 33 minutes under rotating speed 7800r/min, spent Ion water washing 3 times, is produced after freeze-drying.
Embodiment 4
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil, extraction temperature 60 after crushing DEG C, extracting pressure 45MPa, extraction time is 3 hours;
S2:By 0.8g fat-soluble tea polyphenols stirring and dissolving in 10g mackerel fish oil, miscella is obtained;
S3:8g PLAs and miscella are dissolved in 80mL chloroforms and 150mL acetone respectively, and are sufficiently stirred, after blending uniformly It is ultrasonic to obtain dispersed phase;
S4:1g sorbitan oleates, 0.5g polyoxyethylene sorbitol acid anhydride monopalmitates and 1g polyvinyl alcohol are added to In 700mL deionized waters, heating water bath is sufficiently stirred to 95 DEG C and dissolves to obtain continuous phase;
S5:Scattered it will be added in holder, under impressed pressure 0.050MPa effects, by SPG microporous barriers by dispersed phase pressure Enter in continuous phase, obtain monodispersed O/W types emulsion;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, stirred 8 hours with rotating speed 570r/min, with chloroform and acetone Volatilization, be finally solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged 35 minutes under rotating speed 8000r/min, spent Ion water washing 3 times, is produced after freeze-drying.
Comparative example 1
The present embodiment compared with Example 1, does not contain polyoxyethylene sorbitol acid anhydride monopalmitate, is specifically:
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil after crushing, extraction temperature is 45-60 DEG C, extracting pressure 35-45MPa, extraction time is 2-3 hours;
S2:By 0.5-0.8g fat-soluble tea polyphenols stirring and dissolving in 5-10g mackerel fish oil, miscella is obtained;
S3:4-8g PLAs and miscella are dissolved in 50-80mL chloroforms and 100-150mL acetone respectively, and are sufficiently stirred, altogether It is uniformly ultrasonic after mixed to obtain dispersed phase;
S4:0.8-1g sorbitan oleates and 0.5-1g polyvinyl alcohol are added in 500-700mL deionized waters, water-bath 80-95 DEG C is heated to, is sufficiently stirred and dissolves to obtain continuous phase;
S5:It is added to scattered in holder, under impressed pressure 0.045-0.050MPa effects, will be divided by SPG microporous barriers In dephasing press-in continuous phase, monodispersed O/W types emulsion is obtained;
S6:O/W type emulsion is transferred in 15 DEG C of thermostats, 6-8 hours are stirred with rotating speed 520-570r/min, with chloroform With the volatilization of acetone, mackerel fish oil and fat-soluble tea polyphenol complex microsphere are finally solidified into;
S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged into 30-35 under rotating speed 7500-8000r/min Minute, it is washed with deionized 3 times, is produced after freeze-drying.
Comparative example 2
The present embodiment compared with Example 1, does not contain Tea Polyphenols, is specifically:
A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, comprises the following steps:
S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil, extraction temperature 45 after crushing DEG C, extracting pressure 35MPa, extraction time is 2 hours;
S2:4g PLAs and mackerel oil are not dissolved in 50mL chloroforms and 100mL acetone, and are sufficiently stirred, after blending uniformly It is ultrasonic to obtain dispersed phase;
S3:0.8g sorbitan oleates, 0.2g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.5g polyvinyl alcohol are added Enter into 500mL deionized waters, heating water bath is sufficiently stirred to 80 DEG C and dissolves to obtain continuous phase;
S4:Scattered it will be added in holder, under impressed pressure 0.045MPa effects, by SPG microporous barriers by dispersed phase pressure Enter in continuous phase, obtain monodispersed O/W types emulsion;
S5:O/W type emulsion is transferred in 15 DEG C of thermostats, stirred 6 hours with rotating speed 520r/min, with chloroform and acetone Volatilization, be finally solidified into mackerel fish oil and fat-soluble tea polyphenol complex microsphere;
S6:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged 30 minutes under rotating speed 7500r/min, spent Ion water washing 3 times, is produced after freeze-drying.
The partial properties index of mackerel fish oil and fat-soluble tea polyphenol complex microsphere prepared by the present invention see the table below 1, its particle diameter Between 21.43-21.53 μm, load mackerel oil mass is higher, reaches as high as 64.95%, and it is up to 17.44% to carry Tea Polyphenols amount, right 59.98% is up in DPPH clearance rates, inoxidizability is fine, while envelop rate also can reach 19.86%, has and releases well Effect is put, can be absorbed well by enteron aisle.
The partial properties index of the mackerel fish oil of table 1 and fat-soluble tea polyphenol complex microsphere
To in the measure of DPPH clearance rate, microballoon concentration is 5mg/ml.

Claims (4)

  1. A kind of 1. preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere, it is characterised in that:Comprise the following steps:
    S1:Mackerel fish head, freeze-drying is taken to use supercritical carbon dioxide extraction method extraction fish oil after crushing;
    S2:By 0.5-0.8g fat-soluble tea polyphenols stirring and dissolving in 5-10g mackerel fish oil, miscella is obtained;
    S3:4-8g PLAs and miscella are dissolved in 50-80mL chloroforms and 100-150mL acetone respectively, and are sufficiently stirred, altogether It is uniformly ultrasonic after mixed to obtain dispersed phase;
    S4:0.8-1g sorbitan oleates, 0.2-0.5g polyoxyethylene sorbitol acid anhydride monopalmitates and 0.5-1g are gathered Vinyl alcohol is added in 500-700mL deionized waters, and heating water bath is sufficiently stirred to 80-95 DEG C and dissolves to obtain continuous phase;
    S5:It is added to scattered in holder, under impressed pressure 0.045-0.050MPa effects, will be divided by SPG microporous barriers In dephasing press-in continuous phase, monodispersed O/W types emulsion is obtained;
    S6:O/W type emulsion is transferred in 15 DEG C of thermostats, 6-8 hours are stirred with rotating speed 520-570r/min, with chloroform With the volatilization of acetone, mackerel fish oil and fat-soluble tea polyphenol complex microsphere are finally solidified into;
    S7:Mackerel fish oil and fat-soluble tea polyphenol complex microsphere suspension are centrifuged into 30-35 under rotating speed 7500-8000r/min Minute, it is washed with deionized 3 times, is produced after freeze-drying.
  2. 2. the preparation method of a kind of mackerel fish oil according to claim 1 and fat-soluble tea polyphenol complex microsphere, its feature It is:Supercritical extract condition is that extraction temperature is 45-60 DEG C in the S1, extracting pressure 35-45MPa, and extraction time is 2-3 hours.
  3. 3. the preparation method of a kind of mackerel fish oil according to claim 1 and fat-soluble tea polyphenol complex microsphere, its feature It is:Rotating speed is 550r/min in the S6, and mixing time is 7 hours.
  4. 4. the preparation method of a kind of mackerel fish oil according to claim 1 and fat-soluble tea polyphenol complex microsphere, its feature It is:Rotating speed is 7800r/min in the S7, and centrifugation time is 33 minutes.
CN201710934867.8A 2017-10-09 2017-10-09 A kind of preparation method of mackerel fish oil and fat-soluble tea polyphenol complex microsphere Withdrawn CN107510057A (en)

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