CN105176137B - A kind of method for separating and preparing of cape jasmine oily, water-soluble gardenin and Gardenoside - Google Patents
A kind of method for separating and preparing of cape jasmine oily, water-soluble gardenin and Gardenoside Download PDFInfo
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Abstract
The present invention relates to a kind of cape jasmine oil, the method for separating and preparing of water-soluble gardenin and Gardenoside, belong to the development and application field of Natural Medicine Chemistry and food additives.Using cape jasmine seed as raw material, by microwave drying pretreatment, subcritical abstraction, UF membrane, macroporous resin purification and it is dried to obtain cape jasmine oil, gardenin and Gardenoside.The present invention carries out comprehensive comprehensive development and utilization to cape jasmine seed by gradually extracting, and cape jasmine oil, water-soluble cape jasmine and the cape jasmine glycoside product of preparation can be applied to the fields such as food, food additives, health care product, have good commercial promise.
Description
Technical field
The present invention relates to a kind of cape jasmine oil, the method for separating and preparing of water-soluble gardenin and Gardenoside, belong to crude drug
Object, field of food.
Technical background
Cape jasmine seed is the fruit of madder wort cape jasmine (Gardenia jasminoides Ellis), bitter in taste, cold,
It is the important large traditional Chinese medicine of China the effect of reducing fever and causing diuresis, removing pattogenic heat from the blood and toxic material from the body with purging intense heat relieving restlessness.Gardenia Yellow is
A kind of unique water-soluble carotenoids pigment of the nature extracted from cape jasmine fruit, they are pure natural
Pigment, it is nontoxic, highly-safe, there is certain nutritive value and health-care effect, be widely used in medicine, foods and cosmetics etc.
Industry, Gardenia Yellow main component are the α-crocin (α-crocin) and crocetin (crocetin) of carotenoids class.Cape jasmine
Sub- glycosides is the main active of cape jasmine, has the protective effect to liver, pancreatic cell, can promote bile secretion, and
Have the effects that hypoglycemic, decompression, antipyretic, antibacterial, anti-inflammatory, analgesia, anti-oxidant, antitumor, anti-apoptotic and neuroprotection.Cape jasmine
Sub- glycosides is also the important source material for producing Gardenia Blue Pigment.
Currently, the research in China is concentrated mainly on the general Quality Research of gardenin, primarily with respect to Gardenia Yellow
The purification of pigment, the research of functional characteristic and gardenia blue pigment.On the comprehensive development and utilization of cape jasmine raw material, research is owed
It lacks.The present invention is raw material using cape jasmine, using the extraction separation method of no waste, with microwave drying, subcritical mention oil, slightly mentions
Cape jasmine seed oil, Gardenia Yellow and Gardenoside is prepared in the technologies such as object extraction, UF membrane and purification with macroreticular resin simultaneously.
This method greatly reduces the production cost of cape jasmine product, improves the utilization rate of raw material, improves the industrial chain of cape jasmine.
Summary of the invention
To achieve the above object, the method for separating and preparing of a kind of cape jasmine oily, water-soluble gardenin and Gardenoside has been invented,
It is characterized in that comprising the steps of:
First step pretreatment
By fresh cape jasmine seed, shelling, microwave drying is crushed, and is crossed 20-60 mesh, is obtained cape jasmine seed raw material；
The extraction of second step cape jasmine oil
By cape jasmine seed raw material, it is put into extraction kettle, butane injection extraction kettle is mixed with cape jasmine seed raw material, butane and raw material
Mass volume ratio is 1: 5~1: 8 (g: mL), is extracted under conditions of 30~50 DEG C of extraction temperature, 0.6~0.8Mpa of extracting pressure
2~3 times, 0.5~1.0h, after extraction, the butane for carrying cape jasmine seed oil is transported in separating still, is then carried out every time
Be evaporated under reduced pressure, so that butane is sufficiently gasified, in evaporation process control 30~50 DEG C of temperature, etc. butane recoveries it is complete after, from separating still
Bottom releases extracted thick cape jasmine seed oil, and yield is 15~20%, and cape jasmine seed slag is taken out out of extraction kettle；
Third step cape jasmine crude extract extracts
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution, heating and refluxing extraction or reduced-pressure backflow extract or ultrasonic wave assisted extraction or microwave radiation exaraction 1~3 time, every time
10min~8h, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；
4th step UF membrane
By the above-mentioned feed liquid ceramic membrane filter in 0.025 μm~0.2 μm aperture, 0.1~0.4Mpa of pressure will transmit through liquid,
It is recovered under reduced pressure, obtains crude extract feed liquid；
5th step macroporous resin purification
By crude extract feed liquid, with large pore resin absorption column adsorbing separation, mother liquor and macroporous absorbent resin volume ratio (v: v) are
1: 20~1: 50；First being eluted with the ethanol water that mass fraction is 5~15%, amount of eluent is 3~5 times of column volumes,
Eluent I component is obtained, then is eluted with the ethanol water that mass fraction is 20~40%, eluting agent is 2~5 times
Column volume collects eluent II component, is finally eluted with the ethanol water that mass fraction is 50~80%, and eluant, eluent is used
Amount is 4~7 times of column volumes, collects eluent III component；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, warp
It crosses vacuum drying or freeze-drying is Gardenoside；Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, passes through
Vacuum drying or freeze-drying are Gardenia Yellow.
2. the power of microwave drying is 0.1~1.5kW in the first step, it is material bed put down it is auxiliary with a thickness of 5~10cm, when dry
Between be 0.5~2h, dry the moisture content of cape jasmine seed afterwards 5~8%.
3. in third step the temperature of heating and refluxing extraction be 50~90 DEG C, reduced-pressure backflow extract vacuum degree be 0.04~
0.1MPa, 40~70 DEG C of temperature, the power of ultrasound assisted extraction is 120~600W, and temperature is 30~60 DEG C, microwave radiation exaraction
Power be 500~800W, 40~70 DEG C of temperature.
4. the macroporous absorbent resin in the 5th step is selected from LK001,122, polyamide, DM101, AB-8, M1180N and D285
One or more of.
Beneficial effects of the present invention:
The method for separating and preparing of a kind of cape jasmine oily, water-soluble gardenin and Gardenoside provided by the present invention, also has
Following characteristics:
(1) present invention carries out Efficient Development utilization to cape jasmine seed using gradually extracting method, successively obtains cape jasmine oil, Cape jasmine
Sub- glycosides and gardenin, have greatly improved extraction efficiency；
(2) present invention can be effectively prevented Gardenoside and gardenin using extracting methods such as negative pressure, ultrasound and microwaves
The decomposition of extract greatly improves and extracts yield；
(3) present invention process is easy to operate, easily implements, and product quality is high.
Specific embodiment
Following embodiment is some citings of the invention, should not be seen as limitation of the invention.
Embodiment 1
By fresh cape jasmine seed, shelling is material bed to put down auxiliary 5~10cm of thickness in 0.1~1.5kW of microwave drying power, when dry
Between 0.5~2h, the moisture content of cape jasmine seed is 5~8% after having dried.
Embodiment 2
By fresh cape jasmine seed, shelling, microwave drying is crushed, and is crossed 20-60 mesh, is obtained cape jasmine seed raw material, be put into extraction kettle,
Butane injection extraction kettle is mixed with cape jasmine seed raw material, the mass volume ratio of butane and raw material is 1: 5~1: 8 (g: mL), is being extracted
30~50 DEG C of temperature are taken, is extracted 2~3 times under conditions of 0.6~0.8Mpa of extracting pressure, 0.5~1.0h, extraction terminate every time
Afterwards, the butane for carrying cape jasmine seed oil is transported in separating still, is then evaporated under reduced pressure, butane is made sufficiently to gasify, evaporated
Control 30~50 DEG C of temperature in the process, etc. butane recoveries it is complete after, release extracted thick cape jasmine seed oil from separating still bottom, receive
Rate is 15~20%, and cape jasmine seed slag is taken out out of extraction kettle.
Embodiment 3
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution, the temperature of heating and refluxing extraction are 50~90 DEG C, are extracted 1~3 time, 1~8h, filtering, filtrate merge, is configured to every time
The feed liquid that concentration is 2~5%；Then with the ceramic membrane filter in 0.025 μm~0.2 μm aperture, 0.1~0.4Mpa of pressure will be saturating
Liquid is crossed, is recovered under reduced pressure, crude extract feed liquid is obtained；By crude extract feed liquid, with large pore resin absorption column LK001 adsorbing separation,
Mother liquor and macroporous absorbent resin LK001 volume ratio (v: v) are 1: 20~1: 50；The ethanol water for being first 5~15% with mass fraction
Solution is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component, then with mass fraction is 20~40%
Ethanol water is eluted, and eluting agent is 2~5 times of column volumes, is collected eluent II component, is finally with mass fraction
50~80% ethanol water is eluted, and eluting agent is 4~7 times of column volumes, collects eluent III component；Elution
Liquid I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as Gardenoside；Eluent II
It is concentrated under reduced pressure at 40~60 DEG C of temperature and removes ethyl alcohol, by being dried in vacuo or being freeze-dried as Gardenia Yellow.
Embodiment 4
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution, under conditions of 0.04~0.1MPa of vacuum degree that reduced-pressure backflow extracts, 40~70 DEG C of temperature, extraction 1~3 time, often
Secondary 1~3h, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with the pottery in 0.025 μm~0.2 μm aperture
The filtering of porcelain film, 0.1~0.4Mpa of pressure will transmit through liquid, be recovered under reduced pressure, and obtain crude extract feed liquid；By crude extract feed liquid, use
122 adsorbing separation of large pore resin absorption column, mother liquor and 122 volume ratio of macroporous absorbent resin (v: v) are 1: 20~1: 50；First use matter
The ethanol water that amount score is 5~15% is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component, then
It is eluted with the ethanol water that mass fraction is 20~40%, eluting agent is 2~5 times of column volumes, collects eluent
II component is finally eluted with the ethanol water that mass fraction is 50~80%, and eluting agent is 4~7 times of column volumes,
Collect eluent III component；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or freezing
Dry is Gardenoside；Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, dry by being dried in vacuo or freezing
Dry is Gardenia Yellow.
Embodiment 5
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution is 120~600W in the power of ultrasonic wave assisted extraction, under conditions of temperature is 30~60 DEG C, extraction 1~3 time, often
Secondary 10min~40min, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with 0.025 μm~0.2 μm hole
The ceramic membrane filter of diameter, 0.1~0.4Mpa of pressure, will transmit through liquid, is recovered under reduced pressure, and crude extract feed liquid is obtained；By crude extract
Feed liquid is separated with polycaprolactam, and mother liquor and polyamide volume ratio (v: v) are 1: 20~1: 50；First with mass fraction be 5~
15% ethanol water is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component, then use mass fraction
It is eluted for 20~40% ethanol water, eluting agent is 2~5 times of column volumes, collects eluent II component, finally
It is eluted with the ethanol water that mass fraction is 50~80%, eluting agent is 4~7 times of column volumes, collects eluent
III component；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as Cape jasmine
Sub- glycosides；Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as cape jasmine
Uranidin.
Embodiment 6
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution is 500~800W in the power of microwave radiation exaraction, under conditions of 40~70 DEG C of temperature, extracts 1~3 time, every time
10min~40min, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with 0.025 μm~0.2 μm aperture
Ceramic membrane filter, 0.1~0.4Mpa of pressure will transmit through liquid, is recovered under reduced pressure, and obtain crude extract feed liquid；By crude extract material
Liquid, with DM101 adsorbing separation, mother liquor and DM101 volume ratio (v: v) are 1: 20~1: 50；It is first 5~15% with mass fraction
Ethanol water is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component, then with mass fraction for 20~
40% ethanol water is eluted, and eluting agent is 2~5 times of column volumes, is collected eluent II component, is finally used quality
The ethanol water that score is 50~80% is eluted, and eluting agent is 4~7 times of column volumes, collects eluent III group
Part；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as Gardenoside；
Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as cape jasmine yellow
Element.
Embodiment 7
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution, under conditions of 0.04~0.1MPa of vacuum degree that reduced-pressure backflow extracts, 40~70 DEG C of temperature, extraction 1~3 time, often
Secondary 1~3h, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with the pottery in 0.025 μm~0.2 μm aperture
The filtering of porcelain film, 0.1~0.4Mpa of pressure will transmit through liquid, be recovered under reduced pressure, and obtain crude extract feed liquid；By crude extract feed liquid, use
Large pore resin absorption column AB-8 adsorbing separation, mother liquor and macroporous absorbent resin AB-8 volume ratio (v: v) are 1: 20~1: 50；First use
The ethanol water that mass fraction is 5~15% is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component,
It is eluted again with the ethanol water that mass fraction is 20~40%, eluting agent is 2~5 times of column volumes, collects elution
Liquid II component is finally eluted with the ethanol water that mass fraction is 50~80%, and eluting agent is 4~7 times of cylinders
Product collects eluent III component；Eluent I be concentrated under reduced pressure at 40~60 DEG C of temperature remove ethyl alcohol, by vacuum drying or it is cold
Being lyophilized dry is Gardenoside；Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or freezing
Dry is Gardenia Yellow.
Embodiment 8
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution, under conditions of 0.04~0.1MPa of vacuum degree that reduced-pressure backflow extracts, 40~70 DEG C of temperature, extraction 1~3 time, often
Secondary 1~3h, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with the pottery in 0.025 μm~0.2 μm aperture
The filtering of porcelain film, 0.1~0.4Mpa of pressure will transmit through liquid, be recovered under reduced pressure, and obtain crude extract feed liquid；By crude extract feed liquid, use
Large pore resin absorption column M1180N adsorbing separation, mother liquor and macroporous absorbent resin M1180N volume ratio (v: v) are 1: 20~1: 50；
It is first eluted with the ethanol water that mass fraction is 5~15%, amount of eluent is 3~5 times of column volumes, obtains eluent I
Component, then eluted with the ethanol water that mass fraction is 20~40%, eluting agent is 2~5 times of column volumes, is collected
Eluent II component is finally eluted with the ethanol water that mass fraction is 50~80%, and eluting agent is 4~7 times
Column volume collects eluent III component；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by vacuum drying
Or freeze-drying is Gardenoside；Eluent II be concentrated under reduced pressure at 40~60 DEG C of temperature remove ethyl alcohol, by vacuum drying or
Freeze-drying is Gardenia Yellow.
Embodiment 9
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, the ethyl alcohol that mass fraction is 40~80% is added
Aqueous solution is 120~600W in the power of ultrasonic wave assisted extraction, under conditions of temperature is 30~60 DEG C, extraction 1~3 time, often
Secondary 10min~40min, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；Then with 0.025 μm~0.2 μm hole
The ceramic membrane filter of diameter, 0.1~0.4Mpa of pressure, will transmit through liquid, is recovered under reduced pressure, and crude extract feed liquid is obtained；By crude extract
Feed liquid, with D285 adsorbing separation, mother liquor and D285 volume ratio (v: v) are 1: 20~1: 50；It is first 5~15% with mass fraction
Ethanol water is eluted, and amount of eluent is 3~5 times of column volumes, obtains eluent I component, then with mass fraction for 20~
40% ethanol water is eluted, and eluting agent is 2~5 times of column volumes, is collected eluent II component, is finally used quality
The ethanol water that score is 50~80% is eluted, and eluting agent is 4~7 times of column volumes, collects eluent III group
Part；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as Gardenoside；
Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by being dried in vacuo or being freeze-dried as cape jasmine yellow
Element.
Claims (4)
1. the method for separating and preparing of a kind of cape jasmine oil, water-soluble gardenin and Gardenoside, it is characterised in that by following steps group
At:
First step pretreatment
By fresh cape jasmine seed, shelling, microwave drying is crushed, and is crossed 20-60 mesh, is obtained cape jasmine seed raw material；
The extraction of second step cape jasmine oil
By cape jasmine seed raw material, it is put into extraction kettle, butane injection extraction kettle is mixed with cape jasmine seed raw material, the quality of butane and raw material
Volume ratio is 1: 5~1: 8 (mL: g), and 2~3 are extracted under conditions of 30~50 DEG C of extraction temperature, 0.6~0.8MPa of extracting pressure
Secondary, 0.5~1.0h, after extraction, the butane for carrying cape jasmine seed oil is transported in separating still, is then depressurized every time
Evaporation, so that butane is sufficiently gasified, in evaporation process control 30~50 DEG C of temperature, etc. butane recoveries it is complete after, from separating still bottom
Extracted thick cape jasmine seed oil is released, yield is 15~20%, and cape jasmine seed slag is taken out out of extraction kettle；
Third step cape jasmine crude extract extracts
It is 1: 5~1: 30 (g: mL) by mass volume ratio by cape jasmine seed slag, it is water-soluble that the ethyl alcohol that mass fraction is 40~80% is added
Liquid, heating and refluxing extraction or reduced-pressure backflow extract or ultrasonic wave assisted extraction or microwave radiation exaraction 1~3 time, each 10min
~8h, filtering, filtrate merge, and are configured to the feed liquid that concentration is 2%-5%；
4th step UF membrane
By the above-mentioned feed liquid ceramic membrane filter in 0.025 μm~0.2 μm aperture, 0.1~0.4MPa of pressure will transmit through liquid, carry out
It is recovered under reduced pressure, obtains crude extract feed liquid；
5th step macroporous resin purification
By crude extract feed liquid, with large pore resin absorption column adsorbing separation, mother liquor and macroporous absorbent resin volume ratio (v: v) are 1: 20
~1: 50；It is first eluted with the ethanol water that mass fraction is 5~15%, amount of eluent is 3~5 times of column volumes, is obtained
Eluent I component, then eluted with the ethanol water that mass fraction is 20~40%, eluting agent is 2~5 times of cylinders
Product collects eluent II component, is finally eluted with the ethanol water that mass fraction is 50~80%, eluting agent is
4~7 times of column volumes collect eluent III component；Eluent I is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by true
Sky is dry or freeze-drying is Gardenoside；Eluent II is concentrated under reduced pressure at 40~60 DEG C of temperature removes ethyl alcohol, by vacuum
Dry or freeze-drying is Gardenia Yellow.
2. the method for separating and preparing of a kind of cape jasmine oil, water-soluble gardenin and Gardenoside according to claim 1, feature
The power for being microwave drying in the first step is 0.1~1.5kW, and material bed to put down auxiliary with a thickness of 5~10cm, drying time is
0.5~2h, the moisture content of cape jasmine seed is 5~8% after having dried.
3. the method for separating and preparing of a kind of cape jasmine oil, water-soluble gardenin and Gardenoside according to claim 1, feature
The temperature for being heating and refluxing extraction in third step is 50~90 DEG C, and the vacuum degree that reduced-pressure backflow extracts is 0.04~0.1MPa,
40~70 DEG C of temperature, the power of ultrasound assisted extraction is 120~600W, and temperature is 30~60 DEG C, the power of microwave radiation exaraction
For 500~800W, 40~70 DEG C of temperature.
4. the method for separating and preparing of a kind of cape jasmine oil, water-soluble gardenin and Gardenoside according to claim 1, feature
It is one of the macroporous absorbent resin in the 5th step in LK001,122, polyamide, DM101, AB-8, M1180N and D285
Kind is several.
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| CN103387489A (en) * | 2013-07-11 | 2013-11-13 | 苏州大学 | Preparation method of high pure crocin and geniposide |
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