CN107141331A - The extracting method of cholesterol in a kind of marine organisms byproduct - Google Patents
The extracting method of cholesterol in a kind of marine organisms byproduct Download PDFInfo
- Publication number
- CN107141331A CN107141331A CN201710549331.4A CN201710549331A CN107141331A CN 107141331 A CN107141331 A CN 107141331A CN 201710549331 A CN201710549331 A CN 201710549331A CN 107141331 A CN107141331 A CN 107141331A
- Authority
- CN
- China
- Prior art keywords
- cholesterol
- marine organisms
- byproduct
- extracting method
- calcium salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of extracting method of cholesterol in marine organisms byproduct, it includes saponification, into calcium salt, diafiltration, condensing crystallizing, dissolving crystallized, recrystallization, drying and other steps.Non- cholesterol impurity and calcium salt are carried out complexing removal, so as to improve the purity of cholesterol by the present invention into the marine organisms byproduct after saponification is added into calcium chloride in calcium salt step；The present invention carries out continuous diffusion using ketone reagent with ultrasonic wave combination, the dissolution rate of cholesterol can be significantly improved, so as to improve the recovery rate of cholesterol.The cholesterol recovery rate that extracting method of the present invention is obtained is 15 more than 20%, and purity is more than 98%, and process stabilizing, it is easy to industrialize.
Description
Technical field
The present invention relates to a kind of extracting method of cholesterol, and in particular to cholesterol carries in a kind of marine organisms byproduct
Take method.
Background technology
Cholesterol is also referred to as cholesterine, is the indispensable important substance of animal tissue cell, is also with industrial use
Natural materials, there is the extensive market demand, are industrially mainly used in cosmetics, emulsifying agent, medicine etc..It is also calculus bovis factitius, dimension
Raw element D3 and synthetic hormone raw material, cholesterol have liquid crystal property, and solution has mobility, and its molecule can be under certain condition
Lined up regularly as very much, cholesterol from the cholesteryl ester that different aliphatic acid is made is imitated with notable temperature
The liquid crystal material answered.
At present, cholesterol is mainly based on the brain of animal and lanolin extraction, and the method using acetone cold soaking stain is entered
Row is extracted, and this method adds 20 times of amount acetone solns in animal brain dry powder, and time-consuming for dipping（Up to 72 hours）, extract courage and consolidate
Alcohol yield is low（＜ 6%）, purity is low（≤90%）, and toxic organic solvents are remained, institute's extracting substance is only used for feed addictive,
Animal brain resource is caused to waste.And extracting cholesterin from lanolin uses more cumbersome production technology, organic examination used
Agent species is more, and consumption is big, and purity is low and remains toxic organic solvents.
And cholesterol is extracted from marine organisms byproduct and has no report, improve the comprehensive utilization of marine organisms byproduct
Value.
The content of the invention
It is an object of the invention in view of the shortcomings of the prior art, providing a kind of extraction of cholesterol in marine organisms byproduct
Method, the cholesterol recovery rate that this method is obtained is in 15-20%, and purity is more than 98%, and process stabilizing, it is easy to industrialize.
To achieve the above object, the present invention is adopted the following technical scheme that：
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps:（1）Saponification:Weigh ocean
Biological byproduct, then adds sodium hydroxide of 0.2-0.4 times equivalent to marine organisms by-product quality, 0.6-0.8 times pure
Change water and 5-10% lower alcohol, be heated to backflow and start timing, saponification 1.5-2h is cooled to 20-30 DEG C；
（2）Into calcium salt：To step（1）Calcium chloride of 0.2-0.4 times equivalent to saponification liquor quality, side are added in obtained saponification liquor
Edged is stirred, and reaction 30-60min terminates, and removes moisture removal, obtains the calcium salt containing cholesterol；
（3）Diafiltration：Cholesterol calcium salt, plus the 6-8 times of acetone measured are weighed, 30-60min is soaked, it is ultrasonically treated, 2-4h is stood, is put
Go out percolate, repeat the above steps 3-5 times, merge percolate；
（4）Condensing crystallizing：By step（3）The percolate of merging be concentrated under reduced pressure into it is dry, add equivalent to above-mentioned enriched product quality
6-8 times of volume fraction is 90-95% ethanol solution, heats 60-70 DEG C, stirring uses dilute sulphur after being completely dissolved to enriched product
Acid adjusts pH to 1-3, reheats backflow 30-60min, filters while hot, collects filtrate, and crystal is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）The volume fraction that 6-8 times equivalent to crystal mass is added in obtained crystal is 95-
97% ethanol solution, is adjusted after pH to 4-6 with dilute sulfuric acid, plus equivalent to solution quality 0.5-1% hydrogen peroxide, stirring reaction 30-
After 60min, 1-2h is heated to reflux, is filtered, filtrate is collected, cooling down crystallization 8-10h, filtering produces crude product cholesterol；
（6）Recrystallization：The volume fraction that 8-10 times equivalent to crude product cholesterol quality is added into crude product cholesterol is 97-100%
Ethanol solution, and adjust pH to 9-10, be heated to reflux 1-2h, cooling down crystallization, filtering produces fine work cholesterol；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 50-60 DEG C, 1-2h is dried,
Drying temperature is reset for 70-90 DEG C, 2-3h is dried, produces fine work cholesterol finished product.
The extracting method of cholesterol in a kind of described marine organisms byproduct, it is characterised in that：Step（1）Described is low
Level alcohol is one kind in methanol, ethanol or the two mixing.
The extracting method of cholesterol in a kind of described marine organisms byproduct, it is characterised in that：Step（3）Described ketone
Class reagent is one kind in acetone, butanone, cyclohexanone or two kinds of mixing.
The extracting method of cholesterol in a kind of described marine organisms byproduct, it is characterised in that：Step（3）Described is super
Acoustic frequency is 30~50KHz, and temperature adjustment is controlled at 25~35 DEG C, and ultrasonic time is 5-10min.
The extracting method of cholesterol in a kind of described marine organisms byproduct, it is characterised in that：Step（4）And step
（5）Described in dilute sulfuric acid concentration be 10-20%.
Beneficial effects of the present invention:
The present invention by the marine organisms byproduct after saponification into calcium chloride is added in calcium salt step, by non-cholesterol impurity and calcium
Salt carries out complexing removal, so as to improve the purity of cholesterol；The present invention is continuously oozed using ketone reagent with ultrasonic wave combination
Filter, can significantly improve the dissolution rate of cholesterol, so as to improve the recovery rate of cholesterol.The courage that extracting method of the present invention is obtained is consolidated
Alcohol recovery rate is in more than 15-20%, and purity is more than 98%, and process stabilizing, it is easy to industrialize.
Embodiment
Embodiment 1
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 100g is weighed, 20g sodium hydroxide, 60g purified water and 5g first is then added
Alcohol, is heated to backflow and starts timing, saponification 1.5h is cooled to 20 DEG C；
（2）Into calcium salt：To step（1）37g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 30min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 130g, plus 780g acetone, soak 30min, set supersonic frequency as 30KHz, it is warm
Degree regulation control stands 2h, releases percolate, repeat the above steps 3 times, merge percolate after 25 DEG C, ultrasonic 5min；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 42g, adds the 90% of 252g
Ethanol solution, heats 60 DEG C, stirring adjusts pH to 1 after being completely dissolved to enriched product with 10% dilute sulfuric acid, reheats backflow 30min,
Filter while hot, collect filtrate, crystal 35g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）Obtained crystal, adds 210g 95% ethanol solution, and pH is adjusted extremely with 10% dilute sulfuric acid
After 4, plus 1.05g hydrogen peroxide, after stirring reaction 30min, be heated to reflux 1h, filter, collect filtrate, cooling down crystallization 8h,
Filtering produces crude product cholesterol 28g；
（6）Recrystallization：224g 97% ethanol solution is added into crude product cholesterol, and adjusts pH to 9,1h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 20g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 50 DEG C, 2h is dried, resets
Drying temperature is 70 DEG C, dries 3h, produces fine work cholesterol finished product 16.5g.The recovery rate for calculating cholesterol is 16.5%, purity
For 98.2%.
Embodiment 2
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 1kg is weighed, 300g sodium hydroxides, 700g purified water and 80g first is then added
Alcohol, is heated to backflow and starts timing, saponification 2h is cooled to 25 DEG C；
（2）Into calcium salt：To step（1）600g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 50min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 1.3kg, plus 9.1kg butanone, soak 50min, set supersonic frequency as 40KHz,
Temperature adjustment is controlled after 30 DEG C, ultrasonic 7min, stands 3h, is released percolate, is repeated the above steps 4 times, merges percolate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 450g, adds the 93% of 3.15kg
Ethanol solution, heat 65 DEG C, stirring be completely dissolved to enriched product after with 15% dilute sulfuric acid adjust pH to 2, reheat flow back
45min, is filtered while hot, collects filtrate, and crystal 370g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）2.59kg 96% ethanol solution is added in obtained crystal, is adjusted with 15% dilute sulfuric acid
After pH to 5, plus 18.1g hydrogen peroxide, after stirring reaction 40min, be heated to reflux 1.5h, filter, collect filtrate, cooling down knot
Brilliant 9h, filtering produces crude product cholesterol 345g；
（6）Recrystallization：3.1kg 98% ethanol solution is added into crude product cholesterol, and adjusts pH to 9.5, is heated to reflux
1.5h, cooling down crystallization, filtering produces fine work cholesterol 225g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 55 DEG C, 1.5h is dried, then set
Drying temperature is determined for 85 DEG C, is dried 2h, is produced fine work cholesterol finished product 178g.The recovery rate for calculating cholesterol is 17.8%, purity
For 98.3%.
Embodiment 3
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Weigh marine organisms byproduct 100kg, then add 40kg sodium hydroxide, 80kg purified water and
10kg methanol, is heated to backflow and starts timing, saponification 2h is cooled to 30 DEG C；
（2）Into calcium salt：To step（1）80kg calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 60min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 160kg, plus 1280kg cyclohexanone, soak 60min, set supersonic frequency as
50KHz, temperature adjustment is controlled after 35 DEG C, ultrasonic 10min, stands 4h, is released percolate, is repeated the above steps 5 times, merging is oozed
Filtrate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 50kg, adds the 95% of 400kg
Ethanol solution, heat 70 DEG C, stirring be completely dissolved to enriched product after with 20% dilute sulfuric acid adjust pH to 3, reheat flow back
60min, is filtered while hot, collects filtrate, and crystal 40kg is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）320kg 97% ethanol solution is added in obtained crystal, pH is adjusted with 20% dilute sulfuric acid
To after 6, plus 3.2kg hydrogen peroxide, after stirring reaction 60min, be heated to reflux 2h, filter, collect filtrate, cooling down crystallization
10h, filtering produces crude product cholesterol 33kg；
（6）Recrystallization：330kg 100% ethanol is added into crude product cholesterol, and adjusts pH to 10,2h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 26.4kg；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 60 DEG C, 2h is dried, resets
Drying temperature is 90 DEG C, dries 2h, produces fine work cholesterol finished product 20.5kg.The recovery rate for calculating cholesterol is 20.5%, purity
For 99.7%.
Embodiment 4
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 100g is weighed, 20g sodium hydroxide, 60g purified water and 5g second is then added
Alcohol, is heated to backflow and starts timing, saponification 1.5h is cooled to 20 DEG C；
（2）Into calcium salt：To step（1）37g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 30min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 135g, plus 820g acetone, soak 30min, set supersonic frequency as 30KHz, it is warm
Degree regulation control stands 2h, releases percolate, repeat the above steps 3 times, merge percolate after 25 DEG C, ultrasonic 5min；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 45g, adds the 90% of 280g
Ethanol solution, heats 60 DEG C, stirring adjusts pH to 1 after being completely dissolved to enriched product with 10% dilute sulfuric acid, reheats backflow 30min,
Filter while hot, collect filtrate, crystal 37g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）Obtained crystal, adds 222g 95% ethanol solution, and pH is adjusted extremely with 10% dilute sulfuric acid
After 4, plus 1.15g hydrogen peroxide, after stirring reaction 30min, be heated to reflux 1h, filter, collect filtrate, cooling down crystallization 8h,
Filtering produces crude product cholesterol 30g；
（6）Recrystallization：240g 97% ethanol solution is added into crude product cholesterol, and adjusts pH to 9,1h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 24g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 50 DEG C, 2h is dried, resets
Drying temperature is 70 DEG C, dries 3h, produces fine work cholesterol finished product 17.5g.The recovery rate for calculating cholesterol is 17.5%, purity
For 98.1%.
Embodiment 5
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 1kg is weighed, 300g sodium hydroxides, 700g purified water and 80g second is then added
Alcohol, is heated to backflow and starts timing, saponification 2h is cooled to 25 DEG C；
（2）Into calcium salt：To step（1）600g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 50min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 1.4kg, plus 9.8kg butanone, soak 50min, set supersonic frequency as 40KHz,
Temperature adjustment is controlled after 30 DEG C, ultrasonic 7min, stands 3h, is released percolate, is repeated the above steps 4 times, merges percolate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 470g, adds the 93% of 3.29kg
Ethanol solution, heat 65 DEG C, stirring be completely dissolved to enriched product after with 15% dilute sulfuric acid adjust pH to 2, reheat flow back
45min, is filtered while hot, collects filtrate, and crystal 390g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）2.73kg 96% ethanol solution is added in obtained crystal, is adjusted with 15% dilute sulfuric acid
After pH to 5, plus 20.5g hydrogen peroxide, after stirring reaction 40min, be heated to reflux 1.5h, filter, collect filtrate, cooling down knot
Brilliant 9h, filtering produces crude product cholesterol 345g；
（6）Recrystallization：3.1kg 98% ethanol solution is added into crude product cholesterol, and adjusts pH to 9.5, is heated to reflux
1.5h, cooling down crystallization, filtering produces fine work cholesterol 225g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 55 DEG C, 1.5h is dried, then set
Drying temperature is determined for 85 DEG C, is dried 2h, is produced fine work cholesterol finished product 178g.The recovery rate for calculating cholesterol is 17.8%, purity
For 98.8%.
Embodiment 6
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Weigh marine organisms byproduct 100kg, then add 40kg sodium hydroxide, 80kg purified water and
10kg ethanol, is heated to backflow and starts timing, saponification 2h is cooled to 30 DEG C；
（2）Into calcium salt：To step（1）80kg calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 60min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 150kg, plus 1200kg cyclohexanone, soak 60min, set supersonic frequency as
50KHz, temperature adjustment is controlled after 35 DEG C, ultrasonic 10min, stands 4h, is released percolate, is repeated the above steps 5 times, merging is oozed
Filtrate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 52kg, adds the 95% of 400kg
Ethanol solution, heat 70 DEG C, stirring be completely dissolved to enriched product after with 20% dilute sulfuric acid adjust pH to 3, reheat flow back
60min, is filtered while hot, collects filtrate, and crystal 40kg is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）320kg 97% ethanol solution is added in obtained crystal, pH is adjusted with 20% dilute sulfuric acid
To after 6, plus 3.2kg hydrogen peroxide, after stirring reaction 60min, be heated to reflux 2h, filter, collect filtrate, cooling down crystallization
10h, filtering produces crude product cholesterol 33kg；
（6）Recrystallization：330kg 100% ethanol is added into crude product cholesterol, and adjusts pH to 10,2h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 26.4kg；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 60 DEG C, 2h is dried, resets
Drying temperature is 90 DEG C, dries 2h, produces fine work cholesterol finished product 20.5kg.The recovery rate for calculating cholesterol is 20.5%, purity
For 99.3%.
Embodiment 7
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 100g is weighed, then add 20g sodium hydroxide, 60g purified water, 2.5g
Methanol and 2.5 ethanol, are heated to backflow and start timing, saponification 1.5h is cooled to 20 DEG C；
（2）Into calcium salt：To step（1）37g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 30min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 120g, plus 720g acetone, soak 30min, set supersonic frequency as 30KHz, it is warm
Degree regulation control stands 2h, releases percolate, repeat the above steps 3 times, merge percolate after 25 DEG C, ultrasonic 5min；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 40g, adds the 90% of 240g
Ethanol solution, heats 60 DEG C, stirring adjusts pH to 1 after being completely dissolved to enriched product with 10% dilute sulfuric acid, reheats backflow 30min,
Filter while hot, collect filtrate, crystal 33g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）Obtained crystal, adds 200g 95% ethanol solution, and pH is adjusted extremely with 10% dilute sulfuric acid
After 4, plus 1g hydrogen peroxide, after stirring reaction 30min, be heated to reflux 1h, filter, collect filtrate, cooling down crystallization 8h, filtering
Produce crude product cholesterol 26g；
（6）Recrystallization：208g 97% ethanol solution is added into crude product cholesterol, and adjusts pH to 9,1h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 18g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 50 DEG C, 2h is dried, resets
Drying temperature is 70 DEG C, dries 3h, produces fine work cholesterol finished product 15.5g.The recovery rate for calculating cholesterol is 15.5%, purity
For 98.7%.
Embodiment 8
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 1kg is weighed, 300g sodium hydroxides, 700g purified water, 40g methanol is then added
With 40g ethanol, it is heated to backflow and starts timing, saponification 2h is cooled to 25 DEG C；
（2）Into calcium salt：To step（1）600g calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 50min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 1.3kg, plus 9.1kg butanone, soak 50min, set supersonic frequency as 40KHz,
Temperature adjustment is controlled after 30 DEG C, ultrasonic 7min, stands 3h, is released percolate, is repeated the above steps 4 times, merges percolate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 455g, adds the 93% of 3.15kg
Ethanol solution, heat 65 DEG C, stirring be completely dissolved to enriched product after with 15% dilute sulfuric acid adjust pH to 2, reheat flow back
45min, is filtered while hot, collects filtrate, and crystal 360g is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）2.52kg 96% ethanol solution is added in obtained crystal, is adjusted with 15% dilute sulfuric acid
After pH to 5, plus 18.1g hydrogen peroxide, after stirring reaction 40min, be heated to reflux 1.5h, filter, collect filtrate, cooling down knot
Brilliant 9h, filtering produces crude product cholesterol 340g；
（6）Recrystallization：3.1kg 98% ethanol solution is added into crude product cholesterol, and adjusts pH to 9.5, is heated to reflux
1.5h, cooling down crystallization, filtering produces fine work cholesterol 220g；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 55 DEG C, 1.5h is dried, then set
Drying temperature is determined for 85 DEG C, is dried 2h, is produced fine work cholesterol finished product 170g.The recovery rate for calculating cholesterol is 17.0%, purity
For 98.5%.
Embodiment 9
The extracting method of cholesterol in a kind of marine organisms byproduct, it is to prepare according to the following steps：
（1）Saponification:Marine organisms byproduct 100kg is weighed, 40kg sodium hydroxide, 80kg purified water, 5kg is then added
Methanol and 5kg ethanol, be heated to backflow and start timing, saponification 2h is cooled to 30 DEG C；
（2）Into calcium salt：To step（1）80kg calcium chloride is added in obtained saponification liquor, stirring while adding, reaction 60min terminates,
Moisture removal is removed, the calcium salt containing cholesterol is obtained；
（3）Diafiltration：Weigh cholesterol calcium salt 160kg, plus 1280kg cyclohexanone, soak 60min, set supersonic frequency as
50KHz, temperature adjustment is controlled after 35 DEG C, ultrasonic 10min, stands 4h, is released percolate, is repeated the above steps 5 times, merging is oozed
Filtrate；
（4）Condensing crystallizing：By step（3）The percolate of merging is concentrated under reduced pressure into dry paste 46kg, adds the 95% of 368kg
Ethanol solution, heat 70 DEG C, stirring be completely dissolved to enriched product after with 20% dilute sulfuric acid adjust pH to 3, reheat flow back
60min, is filtered while hot, collects filtrate, and crystal 38kg is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）304kg 97% ethanol solution is added in obtained crystal, pH is adjusted with 20% dilute sulfuric acid
To after 6, plus 3.0kg hydrogen peroxide, after stirring reaction 60min, be heated to reflux 2h, filter, collect filtrate, cooling down crystallization
10h, filtering produces crude product cholesterol 35kg；
（6）Recrystallization：350kg 100% ethanol is added into crude product cholesterol, and adjusts pH to 10,2h is heated to reflux, cools
Crystallisation by cooling, filtering produces fine work cholesterol 25.4kg；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 60 DEG C, 2h is dried, resets
Drying temperature is 90 DEG C, dries 2h, produces fine work cholesterol finished product 20.5kg.The recovery rate for calculating cholesterol is 18.8%, purity
For 99.5%.
Claims (5)
1. the extracting method of cholesterol in a kind of marine organisms byproduct, it is characterised in that：It is to prepare according to the following steps：（1）
Saponification:Marine organisms byproduct is weighed, sodium hydroxide of 0.2-0.4 times equivalent to marine organisms by-product quality is then added,
0.6-0.8 times of purified water and 5-10% lower alcohol, are heated to backflow and start timing, saponification 1.5-2h is cooled to 20-
30℃；
（2）Into calcium salt：To step（1）Calcium chloride of 0.2-0.4 times equivalent to saponification liquor quality, side are added in obtained saponification liquor
Edged is stirred, and reaction 30-60min terminates, and removes moisture removal, obtains the calcium salt containing cholesterol；
（3）Diafiltration：Cholesterol calcium salt, plus the 6-8 times of ketone reagent measured are weighed, 30-60min is soaked, it is ultrasonically treated, stand 2-
4h, releases percolate, repeats the above steps 3-5 times, merges percolate；
（4）Condensing crystallizing：By step（3）The percolate of merging be concentrated under reduced pressure into it is dry, add equivalent to above-mentioned enriched product quality
6-8 times of volume fraction is 90-95% ethanol solution, heats 60-70 DEG C, stirring uses dilute sulphur after being completely dissolved to enriched product
Acid adjusts pH to 1-3, reheats backflow 30-60min, filters while hot, collects filtrate, and crystal is collected by filtration in cooling down crystallization；
（5）It is dissolving crystallized：To step（4）The volume fraction that 6-8 times equivalent to crystal mass is added in obtained crystal is 95-
97% ethanol solution, is adjusted after pH to 4-6 with dilute sulfuric acid, plus equivalent to solution quality 0.5-1% hydrogen peroxide, stirring reaction 30-
After 60min, 1-2h is heated to reflux, is filtered, filtrate is collected, cooling down crystallization 8-10h, filtering produces crude product cholesterol；
（6）Recrystallization：The volume fraction that 8-10 times equivalent to crude product cholesterol quality is added into crude product cholesterol is 97-100%
Ethanol solution, and adjust pH to 9-10, be heated to reflux 1-2h, cooling down crystallization, filtering produces fine work cholesterol；
（7）Dry：Fine work cholesterol is put into drying box and is dried, drying temperature is set as 50-60 DEG C, 1-2h is dried,
Drying temperature is reset for 70-90 DEG C, 2-3h is dried, produces fine work cholesterol finished product.
2. the extracting method of cholesterol in a kind of marine organisms byproduct according to claim 1, it is characterised in that：Step
（1）Described lower alcohol is one kind in methanol, ethanol or the two mixing.
3. the extracting method of cholesterol in a kind of marine organisms byproduct according to claim 1, it is characterised in that：Step
（3）Described ketone reagent is one kind in acetone, butanone, cyclohexanone or two kinds of mixing.
4. the extracting method of cholesterol in a kind of marine organisms byproduct according to claim 1, it is characterised in that：Step
（3）Described supersonic frequency is 30~50KHz, and temperature adjustment is controlled at 25~35 DEG C, and ultrasonic time is 5-10min.
5. the extracting method of cholesterol in a kind of marine organisms byproduct according to claim 1, it is characterised in that：Step
（4）And step（5）Described in dilute sulfuric acid concentration be 10-20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710549331.4A CN107141331A (en) | 2017-07-07 | 2017-07-07 | The extracting method of cholesterol in a kind of marine organisms byproduct |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710549331.4A CN107141331A (en) | 2017-07-07 | 2017-07-07 | The extracting method of cholesterol in a kind of marine organisms byproduct |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107141331A true CN107141331A (en) | 2017-09-08 |
Family
ID=59785236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710549331.4A Pending CN107141331A (en) | 2017-07-07 | 2017-07-07 | The extracting method of cholesterol in a kind of marine organisms byproduct |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107141331A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111315855A (en) * | 2017-09-14 | 2020-06-19 | 发酵生物技术有限公司 | Improved method for extracting cholesterol from fish oil waste residue |
| JP2021501737A (en) * | 2017-09-14 | 2021-01-21 | ファーメンタ バイオテク リミテッドＦｅｒｍｅｎｔａ Ｂｉｏｔｅｃｈ Ｌｉｍｉｔｅｄ | Solvent-free method for extracting cholesterol from milk fat |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167717A (en) * | 2011-02-22 | 2011-08-31 | 安徽科宝生物工程有限公司 | Method for extracting cholesterol from animal brain dry powder with ultrasonic waves |
| CN103113446A (en) * | 2013-03-15 | 2013-05-22 | 北京化工大学 | Method for separating and extracting sterol from wool fat |
-
2017
- 2017-07-07 CN CN201710549331.4A patent/CN107141331A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167717A (en) * | 2011-02-22 | 2011-08-31 | 安徽科宝生物工程有限公司 | Method for extracting cholesterol from animal brain dry powder with ultrasonic waves |
| CN103113446A (en) * | 2013-03-15 | 2013-05-22 | 北京化工大学 | Method for separating and extracting sterol from wool fat |
Non-Patent Citations (1)
| Title |
|---|
| 黄娣等: "不同方法提取大海马脂类及脂肪酸组成分析", 《中国海洋药物》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111315855A (en) * | 2017-09-14 | 2020-06-19 | 发酵生物技术有限公司 | Improved method for extracting cholesterol from fish oil waste residue |
| JP2021501737A (en) * | 2017-09-14 | 2021-01-21 | ファーメンタ バイオテク リミテッドＦｅｒｍｅｎｔａ Ｂｉｏｔｅｃｈ Ｌｉｍｉｔｅｄ | Solvent-free method for extracting cholesterol from milk fat |
| JP2021501808A (en) * | 2017-09-14 | 2021-01-21 | ファーメンタ バイオテク リミテッドＦｅｒｍｅｎｔａ Ｂｉｏｔｅｃｈ Ｌｉｍｉｔｅｄ | An improved method of cholesterol extraction from fish oil waste residues |
| EP3625317A4 (en) * | 2017-09-14 | 2021-03-03 | Fermenta Biotech Limited | Improved process for extraction of cholesterol from fish oil waste residue |
| JP7038138B2 (en) | 2017-09-14 | 2022-03-17 | ファーメンタ バイオテク リミテッド | Solvent-free method for extracting cholesterol from milk fat |
| JP7177081B2 (en) | 2017-09-14 | 2022-11-22 | ファーメンタ バイオテク リミテッド | Improved method of extracting cholesterol from fish oil waste residue |
| CN111315855B (en) * | 2017-09-14 | 2023-07-25 | 发酵生物技术有限公司 | Improved method for extracting cholesterol from fish oil waste residue |
| US11718640B2 (en) * | 2017-09-14 | 2023-08-08 | Fermenta Biotech Limited | Process for extraction of cholesterol from fish oil waste residue |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104445276B (en) | A kind of efficient method preparing cyanamide solution | |
| CN107141331A (en) | The extracting method of cholesterol in a kind of marine organisms byproduct | |
| CN108892609A (en) | It is a kind of to prepare the linoleic method of high-purity using safflower seed oil | |
| CN107540657B (en) | Method for treating mother liquor generated in production of 98% imidacloprid raw powder | |
| CN102391186B (en) | Method for preparing ozagrel intermediate (E)-4-(methyl imidazolyl) methyl cinnamate | |
| CN117447427A (en) | Preparation method of furosemide | |
| CN109180532B (en) | High-efficiency preparation method of D-dencichine | |
| CN112457318A (en) | Synthesis process of Reidesciclovir intermediate | |
| CN117105841A (en) | Preparation method of bilirubin | |
| CN107325144B (en) | The extracting method of cholesterol in a kind of lanolin | |
| CN103043640A (en) | Production method of industrial potassium dihydrogen phosphate | |
| CN102167717B (en) | Method for extracting cholesterol from animal brain dry powder with ultrasonic waves | |
| CN107663219A (en) | Troxerutin production method | |
| CN103421043A (en) | Hydrosis process improvement method for synthesizing glyphosate by alkyl ester process | |
| CN112592332A (en) | Preparation process of high-purity nicotine | |
| CN111808018A (en) | Production process of acetamiprid | |
| CN112480037B (en) | Synthesis method of diphenhydrasol hydrochloride | |
| CN103483376A (en) | Technology of extracting co-produced fytic acid and nicotine from tobacco waste | |
| CN107043343A (en) | A kind of preparation method of L pyroglutamic acids | |
| CN108409711A (en) | The preparation method of 2- thenoyl hydrazines | |
| CN108440334A (en) | A method of preparing 3,4,5- trimethoxybenzoyl hydrazines | |
| CN104788348A (en) | Method for extracting natural taurine from pearl shells | |
| CN108409598A (en) | A method of preparing salicylyl hydrazine | |
| CN117945434A (en) | Method for recycling ammonium sulfate from pymetrozine intermediate aldehyde pyridine wastewater | |
| CN113943338A (en) | Method for extracting tigogenin from sisal dregs and preparing fertilizer from sisal dregs |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170908 |