CN109603201A - The minimizing technology of benzoic acid in pepper extract - Google Patents
The minimizing technology of benzoic acid in pepper extract Download PDFInfo
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Abstract
The minimizing technology of benzoic acid in a kind of pepper extract comprising following steps: (1) being added alcohol solution in pepper extract, after stirring and evenly mixing under the conditions of 41~50 DEG C, stratification, upper layer obtains solution II, and lower layer obtains solution I；(2) solution I removes organic solvent to get the pepper extract I of benzoic acid qualification；(3) it is 80~85% that the solution II, which is added low concentration alcohol aqueous solution and is diluted to alcohol content, adjusts pH≤2, macroporous absorbent resin is crossed after heating, collected column liquid；(4) pure water is added to alcohol content≤10% in the column liquid of crossing, and adjusts pH value to 7~10, after stirring and evenly mixing, after centrifugation removal water layer, removes organic solvent, obtain the pepper extract II of benzoic acid qualification.The present invention can make the removal rate of benzoic acid in pepper extract reach maximization, and simple process and low cost by organic solvent method and Flavonoids by Macroporous Adsorption Resin, be suitable for industrialized production.
Description
Technical field
The invention belongs to the removal technology fields of hazardous material in natural extract, and in particular to benzene in a kind of pepper extract
The minimizing technology of formic acid.
Background technique
Benzoic acid is widely used as food preservative, but excess, long-term consumption meeting harmful to human liver, renal function, because
This, there are stringent limitation in countries in the world to the content of benzoic acid in food and food additives, also define in China's national standard
The maximum usage amount (200-1500mg/kg) of benzoic acid in 22 based foods is defined, is not allowed in the food in addition to this 22 class
Benzoic acid is added as preservative.
But has the secondary metabolite that more document report benzoic acid are plant at present, it is a variety of to be naturally present in capsicum etc.
In plant.Pepper extract is to extract to obtain from capsicum, and in the production processes such as extraction, concentration, benzoic acid is transferred, is rich
Collect in pepper extract so that pepper extract it is a large amount of, be widely used there is food safety hazards, influence capsicum extraction
The sound development of produce industry.Therefore the minimizing technology of benzoic acid is very necessary in exploitation pepper extract.
Currently, the document report about removal benzoic acid is primarily directed to industrial wastewater, removal technology mainly includes life
Object charcoal, anionic surfactant and aluminium salt adsorb micella flocculation, macroporous absorbent resin, modified alta-mud, enzyme preparation etc., not yet
There is the minimizing technology of benzoic acid in document report pepper extract.Pepper extract is capsochrome, capsaicine and oleo resin capsicum
Mixture, target component stability is poor, thus seek it is a kind of not only can be with industrialized production, but also do not influence target component yield
The minimizing technology of benzoic acid is a technical problem to be solved urgently.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of minimizing technologies of benzoic acid in pepper extract, do not influence mesh
The benzoic acid in removal pepper extract is maximized under conditions of mark ingredient yield.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: benzoic acid goes in a kind of pepper extract
Except method, comprising the following steps:
(1) alcohol solution is added in pepper extract, after stirring and evenly mixing under the conditions of 41~50 DEG C, stratification, upper layer obtains molten
Liquid II, lower layer obtain solution I；
(2) organic solvent is removed through deodorization pot under the solution I, obtains the pepper extract I of benzoic acid qualification；
(3) it is 80~85% that the solution II, which is added low concentration alcohol aqueous solution and is diluted to alcohol content, adjusts pH≤2, it is heated to 41~
After 50 DEG C, macroporous absorbent resin is crossed, column liquid was collected；
(4) pure water is added to alcohol content≤10% in the column liquid of crossing, and lye is added and adjusts pH value to 7~10, after stirring and evenly mixing, from
Heart layering after removing water layer, removes organic solvent through deodorization pot, obtains the pepper extract II of benzoic acid qualification.
Step (1) alcohol solution is the methanol aqueous solution or ethanol water that volume ratio is 91:9~95:5, capsicum
The mass volume ratio of extract and alcohol solution is 1:3~4；
Step (3) the low concentration alcohol aqueous solution is the methanol aqueous solution or ethanol water that volume ratio is 5:95~20:80；Institute
Stating macroporous absorbent resin is NKA-II, SD300 or XDA-1, and adsorption flow rate is 1~3BV/h；Adjusting solution used in pH value is matter
Measure the aqueous citric acid solution of score 1~5 ‰.
Step (4) lye is the sodium hydroxide solution or sodium bicarbonate solution that mass fraction is 1~3 ‰；Centrifugation is set
Standby is Horizontal helical type centrifuge, separation factor 6000.
The temperature that the step (2), step (4) remove organic solvent is 45~50 DEG C, vacuum degree >=0.085MPa；It deodorizes
The stirring rate of pot is 60~80r/min.
Beneficial effect by adopting the above technical scheme is: (1) pepper extract precipitated and separated is made by alcohol solution,
While obtaining the pepper extract I of benzoic acid qualification, separate the target component in pepper extract；(2) it is inhaled by macropore
The synergy of attached resin method and organic solvent method, the removal rate of benzoic acid reaches maximization in pepper extract II；(3) column is crossed
Pure water is added in liquid, pepper extract is precipitated, not only ensure that the yield of pepper extract, but also to can remove water solubility therein miscellaneous
Matter improves product quality；It (4), can be after sodium hydroxide solution zeolite regeneration after macroporous absorbent resin Adsorption of Benzoic Acid saturation
It reuses, reduces removal cost；(5) present invention process is simple, at low cost, is suitable for industrialized production.
Specific embodiment
The present invention will be further described in detail combined with specific embodiments below.
Embodiment 1
(1) ethanol water that 60L volume ratio is 91:9 is added into 20kg pepper extract, is stirred and evenly mixed under the conditions of 50 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 45 DEG C of vacuum degree 0.085MPa, the deodorization pot through revolving speed 70r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 80% that the ethanol water that acquired solution II is added that volume ratio is 5:95, which is diluted to ethanol content, and mass fraction is added
PH≤2 are adjusted for 1 ‰ aqueous citric acid solutions, after being heated to 45 DEG C, NKA-II macroporous absorption tree is crossed with the adsorption flow rate of 1BV/h
Rouge collected column liquid；
(4) it is 8% that gained, which crosses column liquid and pure water to ethanol content is added, adds the sodium hydroxide solution that mass fraction is 1 ‰ and adjusts
PH value after stirring and evenly mixing, is centrifuged layering through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer, at 45 DEG C to 7.0
Deodorization pot under the conditions of vacuum degree 0.085MPa through revolving speed 70r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification is extracted
Object II.
Through detecting, the content of benzoic acid is 24.2mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 2
(1) methanol aqueous solution that 70L volume ratio is 95:5 is added into 20kg pepper extract, is stirred and evenly mixed under the conditions of 45 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 47 DEG C of vacuum degree 0.090MPa, the deodorization pot through revolving speed 80r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 82% that the methanol aqueous solution that acquired solution II is added that volume ratio is 10:90, which is diluted to methanol content, and quality point is added
Number is that 2 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 50 DEG C, crosses SD300 macroporous absorption tree with the adsorption flow rate of 2BV/h
Rouge collected column liquid；
(4) gained crosses column liquid, and it is 7% that pure water to methanol content, which is added, adds the sodium bicarbonate solution tune that mass fraction is 3 ‰
PH value is saved to 7.5, after stirring and evenly mixing, layering is centrifuged through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer, 47
Deodorization pot under the conditions of DEG C vacuum degree 0.090MPa through revolving speed 80r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification mentions
Take object II.
Through detecting, the content of benzoic acid is 23.5mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 3
(1) ethanol water that 80L volume ratio is 93:7 is added into 20kg pepper extract, is stirred and evenly mixed under the conditions of 41 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 50 DEG C of vacuum degree 0.095MPa, the deodorization pot through revolving speed 60r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 85% that the ethanol water that acquired solution II is added that volume ratio is 20:80, which is diluted to ethanol content, and quality point is added
Number is that 5 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 48 DEG C, crosses XDA-1 macroporous absorption tree with the adsorption flow rate of 3BV/h
Rouge collected column liquid；
(4) gained crosses column liquid, and it is 9% that pure water to ethanol content, which is added, adds the sodium bicarbonate solution tune that mass fraction is 2 ‰
PH value is saved to 8.0, after stirring and evenly mixing, layering is centrifuged through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer, 50
Deodorization pot under the conditions of DEG C vacuum degree 0.095MPa through 60r/min removes organic solvent, obtains the pepper extract of benzoic acid qualification
II。
Through detecting, the content of benzoic acid is 25.0mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 4
(1) methanol aqueous solution that 400L volume ratio is 92:8 is added into 100kg pepper extract, is stirred and evenly mixed under the conditions of 44 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 47 DEG C of vacuum degree 0.090MPa, the deodorization pot through revolving speed 65r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 82% that the methanol aqueous solution that acquired solution II is added that volume ratio is 8:92, which is diluted to methanol content, and mass fraction is added
PH≤2 are adjusted for 3 ‰ aqueous citric acid solutions, after being heated to 42 DEG C, XDA-1 macroporous adsorbent resin is crossed with the adsorption flow rate of 1.5BV/h,
Collected column liquid；
(4) gained crosses column liquid, and it is 10% that pure water to methanol content, which is added, adds the sodium bicarbonate solution that mass fraction is 1.5 ‰
PH value is adjusted to 8.5, after stirring and evenly mixing, is centrifuged layering through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer,
Deodorization pot under the conditions of 50 DEG C of vacuum degree 0.085MPa through revolving speed 65r/min removes organic solvent, obtains the capsicum of benzoic acid qualification
Extract II.
Through detecting, the content of benzoic acid is 25.8mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 5
(1) methanol aqueous solution that 380L volume ratio is 93:7 is added into 100kg pepper extract, is stirred and evenly mixed under the conditions of 50 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 46 DEG C of vacuum degree 0.095MPa, the deodorization pot through revolving speed 75r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 83% that the methanol aqueous solution that acquired solution II is added that volume ratio is 17:83, which is diluted to methanol content, and quality point is added
Number is that 2 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 45 DEG C, crosses SD300 macroporous absorption tree with the adsorption flow rate of 1BV/h
Rouge collected column liquid；
(4) gained crosses column liquid, and it is 3% that pure water to methanol content, which is added, adds the sodium hydroxide solution tune that mass fraction is 2 ‰
PH value is saved to 9.0, after stirring and evenly mixing, layering is centrifuged through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer, 46
Deodorization pot under the conditions of DEG C vacuum degree 0.095MPa through revolving speed 80r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification mentions
Take object II.
Through detecting, the content of benzoic acid is 22.6mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 6
(1) ethanol water that 160L volume ratio is 95:5 is added into 50kg pepper extract, is stirred and evenly mixed under the conditions of 48 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 47 DEG C of vacuum degree 0.10MPa, the deodorization pot through revolving speed 78r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 85% that the ethanol water that acquired solution II is added that volume ratio is 20:80, which is diluted to ethanol content, and quality point is added
Number is that 1 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 47 DEG C, crosses SD300 macroporous absorption with the adsorption flow rate of 2.5BV/h
Resin collected column liquid；
(4) gained crosses column liquid, and it is 2% that pure water to ethanol content, which is added, adds the sodium bicarbonate solution tune that mass fraction is 1 ‰
PH value is saved to 9.5, after stirring and evenly mixing, layering is centrifuged through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer, 48
Deodorization pot under the conditions of DEG C vacuum degree 0.090MPa through revolving speed 62r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification mentions
Take object II.
Through detecting, the content of benzoic acid is 23.3mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 7
(1) ethanol water that 180L volume ratio is 94:6 is added into 50kg pepper extract, is stirred and evenly mixed under the conditions of 46 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 50 DEG C of vacuum degree 0.090MPa, the deodorization pot through revolving speed 62r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 83% that the ethanol water that acquired solution II is added that volume ratio is 12:88, which is diluted to methanol content, and quality point is added
Number is that 4 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 41 DEG C, crosses XDA-1 macroporous absorption tree with the adsorption flow rate of 1BV/h
Rouge collected column liquid；
(4) gained crosses column liquid, and it is 10% that pure water to methanol content, which is added, adds the sodium hydroxide solution tune that mass fraction is 3 ‰
PH value is saved to 10.0, after stirring and evenly mixing, is centrifuged layering through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer,
Deodorization pot under the conditions of 45 DEG C of vacuum degree 0.095MPa through revolving speed 77r/min removes organic solvent, obtains the capsicum of benzoic acid qualification
Extract II.
Through detecting, the content of benzoic acid is 25.4mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 8
(1) methanol aqueous solution that 75L volume ratio is 91:9 is added into 20kg pepper extract, is stirred and evenly mixed under the conditions of 45 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 48 DEG C of vacuum degree 0.085MPa, the deodorization pot through revolving speed 60r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 84% that the methanol aqueous solution that acquired solution II is added that volume ratio is 15:85, which is diluted to methanol content, and quality point is added
Number is that 3 ‰ aqueous citric acid solutions adjust pH≤2, after being heated to 43 DEG C, crosses NKA-II macroporous absorption with the adsorption flow rate of 2.5BV/h
Resin collected column liquid；
(4) gained crosses column liquid, and it is 2.5% that pure water to methanol content, which is added, adds the sodium bicarbonate solution that mass fraction is 5 ‰
PH value is adjusted to 8.0, after stirring and evenly mixing, is centrifuged layering through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer,
Deodorization pot under the conditions of 46 DEG C of vacuum degree 0.10MPa through revolving speed 70r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification mentions
Take object II.
Through detecting, the content of benzoic acid is 21.2mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Embodiment 9
(1) methanol aqueous solution that 330L volume ratio is 94:6 is added into 100kg pepper extract, is stirred and evenly mixed under the conditions of 42 DEG C
Afterwards, layering is staticly settled, upper layer obtains solution II, and lower layer obtains solution I；
(2) for acquired solution I under the conditions of 48 DEG C of vacuum degree 0.085MPa, the deodorization pot through revolving speed 66r/min removes organic solvent,
Obtain pepper extract I；
(3) it is 82% that the methanol aqueous solution that acquired solution II is added that volume ratio is 7:93, which is diluted to methanol content, and mass fraction is added
PH≤2 are adjusted for 5 ‰ aqueous citric acid solutions, after being heated to 50 DEG C, NKA-II macroporous absorption tree is crossed with the adsorption flow rate of 2BV/h
Rouge collected column liquid；
(4) gained crosses column liquid, and it is 6% that pure water to methanol content, which is added, adds the sodium hydroxide solution that mass fraction is 2.5 ‰
PH value is adjusted to 9.0, after stirring and evenly mixing, is centrifuged layering through the Horizontal helical type centrifuge that separation factor is 6000, after removing water layer,
Deodorization pot under the conditions of 47 DEG C of vacuum degree 0.10MPa through revolving speed 80r/min removes organic solvent, and the capsicum for obtaining benzoic acid qualification mentions
Take object II.
Through detecting, the content of benzoic acid is 24.9mg/kg in raw material pepper extract, and the capsicum after removing benzoic acid is extracted
Benzoic acid is not detected in object I and pepper extract II, method detection is limited to 2mg/kg.
Claims (4)
1. the minimizing technology of benzoic acid in pepper extract, which is characterized in that itself the following steps are included:
(1) alcohol solution is added in pepper extract, after stirring and evenly mixing under the conditions of 41~50 DEG C, stratification, upper layer obtains molten
Liquid II, lower layer obtain solution I；
(2) organic solvent is removed through deodorization pot under the solution I, obtains the pepper extract I of benzoic acid qualification；
(3) it is 80~85% that the solution II, which is added low concentration alcohol aqueous solution and is diluted to alcohol content, adjusts pH≤2, it is heated to 41~
After 50 DEG C, macroporous absorbent resin is crossed, column liquid was collected；
(4) pure water is added to alcohol content≤10% in the column liquid of crossing, and lye is added and adjusts pH value to 7~10, after stirring and evenly mixing, from
Heart layering after removing water layer, removes organic solvent through deodorization pot, obtains the pepper extract II of benzoic acid qualification；
Step (1) alcohol solution is the methanol aqueous solution or ethanol water that volume ratio is 91:9~95:5, and capsicum is extracted
The mass volume ratio of object and alcohol solution is 1:3~4；
Step (3) the low concentration alcohol aqueous solution is the methanol aqueous solution or ethanol water that volume ratio is 5:95~20:80；Institute
Stating macroporous absorbent resin is NKA-II, SD300 or XDA-1, and adsorption flow rate is 1~3BV/h；
Step (4) lye is the sodium hydroxide solution or sodium bicarbonate solution that mass fraction is 1~3 ‰；
The temperature that the step (2), step (4) remove organic solvent is 45~50 DEG C, vacuum degree >=0.085MPa.
2. the minimizing technology of benzoic acid in pepper extract according to claim 1, which is characterized in that the step (2),
The stirring rate of step (4) deodorization pot is 60~80r/min.
3. the minimizing technology of benzoic acid in pepper extract according to claim 1, which is characterized in that the step (3)
PH value is adjusted using the aqueous citric acid solution of mass fraction 1~5 ‰.
4. the minimizing technology of benzoic acid in pepper extract according to claim 1,2 or 3, which is characterized in that the step
Suddenly (4) centrifugation apparatus is Horizontal helical type centrifuge, separation factor 6000.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114195665A (en) * | 2021-12-14 | 2022-03-18 | 武汉世吉药业有限公司 | Neutralization and acidification process and equipment for high-purity NCAA |
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