CN104522264A - Method for preparing cocoa butter equivalent by utilizing palm oil intermediate fractionation product enzymatic transesterfication - Google Patents
Method for preparing cocoa butter equivalent by utilizing palm oil intermediate fractionation product enzymatic transesterfication Download PDFInfo
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- CN104522264A CN104522264A CN201410823600.8A CN201410823600A CN104522264A CN 104522264 A CN104522264 A CN 104522264A CN 201410823600 A CN201410823600 A CN 201410823600A CN 104522264 A CN104522264 A CN 104522264A
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Abstract
The invention discloses a method for preparing a cocoa butter equivalent by utilizing palm oil intermediate fractionation product enzymatic transesterfication. The method comprises the following steps: mixing a palm oil intermediate fractionation product with stearic acid according to a certain mass ratio, carrying out an esterification reaction by virtue of specific lipase to prepare the cocoa butter equivalent, and purifying the product by virtue of two-step crystallizing fractionation. By utilizing the method for preparing the cocoa butter equivalent disclosed by the invention, the produced cocoa butter equivalent is high in similarity with natural cocoa butter and is low in cost and high in safety.
Description
Technical field
The present invention relates to a kind of cacaolike butter preparation method, particularly a kind ofly utilize fraction leach-s/tive enzymic transesterification in the middle of palm oil to prepare the method for cacaolike butter.
Background technology
Cocoa butter (
cocoa butter) also known as cocoa butter, be from tropical plants cocoa chocolate tree (Theobroma cacao) seed cocoa bean in extract the faint yellow rigid natural plant grease having unique perfume obtained.Cocoa bean main product is in torrid areas, regional within being mainly north and south, equator 20 latitude.The output of whole world cocoa bean in 2013 is 5,000,000 tons, and wherein Africa accounts for 65.7%, and Asia accounts for 19.2%, and America accounts for 14.2%, and Oceania accounts for 0.9%.Due to local flavor and the pre-arcing characterisitics of cocoa butter uniqueness, cocoa butter is widely used in the food manufacturing industries such as chocolate, candy coat and dessert.
The main fatty acid of cocoa butter consists of: palmitic acid 24.2% ~ 27.0%, stearic acid 32.6% ~ 35.4%, oleic acid 33.8% ~ 36.9%, linoleic acid 2.7% ~ 3.54%.Containing a certain amount of tocopherol in cocoa butter, its content is about 230mg/kg, and wherein 85% is Gamma-Tocopherol; The polyunsaturated fatty acid of adding cocoa butter, than seldom, makes cocoa butter have very strong oxidation resistance, long shelf-life.
What main and its aliphatic acid of the physical characteristic of cocoa butter uniqueness formed particularly triglycerides is configured with much relations, cocoa butter mainly Sn-2 position is that saturated-2 unsaturated triglycerides of symmetric form 1,3 (β-POP+ β-POSt+ β-StOSt) of oleic acid are higher than 75%.In cocoa butter 1,3-bis-palmityl-2-oleoyl glyceride (POP) content is about 12%, 1-palmityl-2-oleoyl-3-palmitostearate (POSt) content is about 48%, 1,3-distearyl-2-oleoyl glyceride (StOSt) content about 26%.
Cocoa butter mainly originates in torrid areas, and owing to being subject to geographical position and climatic influences, its output can not meet the demand of food industry far away.At present, the countries and regions such as European Union and the U.S. have allowed in chocolate, add the cocoa butter replacers being no more than 5%.By hydrogenation, point to carry, cheap, common edible oil and fat are processed into cocoa butter in physical characteristic by the oil and fat modification technology people such as ester exchange, particularly similar with cocoa butter on melting range product.Easily produce harmful trans acids in hydrogenation process, not only output is few for point cocoa butter replacers raised, and mouthfeel and quality and natural cocoa butter have larger gap.Before the nineties in 20th century, high-quality cocoa butter product is mainly in developed country's area consumption such as America and Europes, along with economic fast developments of populous nation such as China, India, the market demand of cocoa butter sharply increases, and the output of natural cocoa butter can not meet the demand in market far away.
Summary of the invention
The object of the invention is to provide a kind of palm oil middle fraction leach-s/tive enzymic transesterification legal system that utilizes for the method for cacaolike butter.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of palm oil middle fraction leach-s/tive enzymic transesterification legal system that utilizes is for the method for cacaolike butter, it is characterized in that the concrete steps of the method are as follows: be dissolved in n-hexane by fraction leach-s/tive in the middle of palm oil and stearic acid by the mass ratio of 1:0.75 ~ 1.5, under temperature is 50-65 DEG C of condition, stirring reaction 150 ~ 180 minutes, finally add the enzyme of 8% ~ 12% of fraction leach-s/tive and stearic acid gross mass in the middle of palm oil, filter while hot after reaction terminates, obtain filtrate, n-hexane is added in this filtrate, place and filter in 0 ~ 4 DEG C of environment 4 ~ 6 hours, after filtrate removes solvent, be dissolved in acetone, to place in 0 ~ 4 DEG C of environment 6 ~ 8 hours, collected by filtration and cacaolike butter, described n-hexane is 10L:1kg with the volume mass ratio of substrate, described acetone is 10L:1kg with the volume mass ratio of substrate.
In the middle of above-mentioned palm oil, fraction leach-s/tive is: palm oil raises fusing point at the grease of 24-28 DEG C through freezing point.
Above-mentioned enzyme is the lipase and immobilised enzymes thereof that produce in rhizomucor miehei bacterium or the thermophilic hyphomycete of thin cotton like.
The method preparing cacaolike butter of the present invention, the aliphatic acid composition of the cacaolike butter produced, the distribution of triglycerides, hot property and hard fat acid content etc. are all very similar to natural cocoa butter, and yield is high, and cost is low.
Accompanying drawing explanation
Fig. 1 is the DSC figure of natural cocoa butter.
Fig. 2 is the DSC figure of the crystallization of cacaolike butter prepared by the inventive method.
Detailed description of the invention
Embodiment one: a kind of chemically catalyzed interesterification legal system that utilizes is for the method for cacaolike butter, comprise the following steps: getting mass ratio is that in the middle of the palm oil of 4 grams: 4 grams, fraction leach-s/tive and stearic acid mixing are placed in reaction there-necked flask, at 50 DEG C, mixing speed is 300r/min, add the immobilized lipase 0.8g that the thermophilic hyphomycete of thin cotton like produces, react 150 minutes; Filter while hot, add 80ml n-hexane, be placed in 4 DEG C of refrigerators and filter after 4 hours, rotary evaporation adds 80ml acetone after removing solvent again, and be placed in 4 DEG C of refrigerators and filter for 8 hours, collect the crystallized product obtained, rotary evaporation is removed residual solvent and namely obtained cacaolike butter.
Embodiment two: a kind of chemically catalyzed interesterification legal system that utilizes is for the method for cacaolike butter, comprise the following steps: getting mass ratio is that in the middle of the palm oil of 40 grams: 40 grams, fraction leach-s/tive and stearic acid mixing are placed in reaction there-necked flask, at 60 DEG C, mixing speed is 300r/min, add the immobilized lipase 8.0g that the thermophilic hyphomycete of thin cotton like produces, react 150 minutes; Filter while hot, add 800ml n-hexane, be placed in 4 DEG C of refrigerators and filter after 4 hours, rotary evaporation adds 800ml acetone after removing solvent again, be placed in 4 DEG C of refrigerators to filter for 8 hours, collect the crystallized product obtained, rotary evaporation is removed residual solvent and is namely obtained cacaolike butter.
Embodiment three: a kind of chemically catalyzed interesterification legal system that utilizes is for the method for cacaolike butter, comprise the following steps: getting mass ratio is that in the middle of the palm oil of 40 grams: 40 grams, fraction leach-s/tive and stearic acid mixing are placed in reaction there-necked flask, at 50 DEG C, mixing speed is 300r/min, add the immobilized lipase 8.0g that the thermophilic hyphomycete of thin cotton like produces, react 180 minutes; Filter while hot, add 800ml n-hexane, be placed in 4 DEG C of refrigerators and filter after 4 hours, rotary evaporation adds 800ml acetone after removing solvent again, be placed in 4 DEG C of refrigerators to filter for 8 hours, collect the crystallized product obtained, rotary evaporation is removed residual solvent and is namely obtained cacaolike butter.
Product checking:
The detection of aliphatic acid:
20mg sample is weighed in 10ml tool plug test tube with electronic analytical balance, add 2.5ml n-hexane, add 1ml and obtain 0.5M sodium methoxide solution, jog 5 minutes under room temperature, then a small amount of anhydrous sodium sulfate is added, to leave standstill after 1 hour under 2000 ~ 3000rpm centrifugal 2 ~ 3 minutes, supernatant liquor is used for gas chromatographic analysis.
Gas-chromatography coupling hydrogen ion flame detector (GC-FID) is adopted to analyze aliphatic acid composition.Chromatographic column is Agilent DB-5MS, 30m × 0.25mm, 0.50 μm, carrier gas: nitrogen, vaporizer temperature: 250 DEG C, detector temperature: 260 DEG C, column temperature: 180 DEG C (2min)-240 DEG C (2 DEG C/min) (5min), sample size: 5 μ l.
The detection of triglycerides:
Weigh 20mg sample in ground conical flask with electronic analytical balance, add 20ml liquid chromatogram absolute dichloromethane, seal and wait to try.High performance liquid chromatography coupling EISD (HPLC-ELSD) is adopted to analyze.Chromatographic column is Agilent ZORBAX SB-C18 post, 250 × 4.6 mm, 5 μm, and mobile phase is acetonitrile and carrene (gradient elution program is in table 1), column temperature 20 DEG C, and flow velocity is 1.0 mL/min, and sampling volume is 5 μ l.EISD optimum configurations is, drift tube temperature is 65 DEG C, nitrogen flow 1.8L/min, and signal amplification factor is 1, selects ram "Off" pattern.
Table 1. HPLC condition of gradient elution
Heat property test:
Accurately take sample 8-10 mg, the crystallization curve under adopting differential calorimetric scan instrument to measure different rate of temperature fall.Temperature control program: sample is heated to 80 DEG C with the heating rate of 20 DEG C/min and keeps 10 min to eliminate crystallization memory, again respectively with 1, the rate of temperature fall of 5,10 and 20 DEG C/min is down to-20 DEG C, the exotherm in record crystallization process.
The cacaolike butter prepared as can be seen from Table 2 and the aliphatic acid of natural cocoa butter form and triglycerides forms all closely similar, and the hot property of the cacaolike butter prepared and natural cocoa butter is also closely similar.
The aliphatic acid of the cacaolike butter of table 2. natural cocoa butter and preparation and the composition of triglycerides
Note: POP, 1,3-bis-palmitic acid-2-oleic three ester; POS, 1-palmitic acid 2-oleic acid-3 glycerol stearate three ester; SOS, 1,3-distearyl acid-2-oleic three ester.
Claims (3)
1. one kind utilizes palm oil middle fraction leach-s/tive enzymic transesterification legal system for the method for cacaolike butter, it is characterized in that the concrete steps of the method are as follows: be dissolved in n-hexane by fraction leach-s/tive in the middle of palm oil and stearic acid by the mass ratio of 1:0.75 ~ 1.5, under temperature is 50-60 DEG C of condition, stirring reaction 150 ~ 180 minutes, finally add the enzyme of 8% ~ 10% of fraction leach-s/tive and stearic acid gross mass in the middle of palm oil, filter while hot after reaction terminates, obtain filtrate, n-hexane is added in this filtrate, place and filter in 0 ~ 4 DEG C of environment 4 ~ 6 hours, after filtrate removes solvent, be dissolved in acetone, to place in 0 ~ 4 DEG C of environment 6 ~ 8 hours, collected by filtration and cacaolike butter, described n-hexane is 10L:1kg with the volume mass ratio of substrate, described acetone is 10L:1kg with the volume mass ratio of substrate.
2. according to claim 1ly utilize in the middle of palm oil that fraction leach-s/tive enzymic transesterification legal system is for the method for cacaolike butter, in the middle of it is characterized in that described palm oil, fraction leach-s/tive is: palm oil raises fusing point at the grease of 24-28 DEG C through freezing point.
3. the fraction leach-s/tive enzymic transesterification legal system that to utilize in the middle of palm oil according to claim 1 is for the method for cacaolike butter, it is characterized in that described enzyme is the lipase and immobilised enzymes thereof that produce in rhizomucor miehei bacterium or the thermophilic hyphomycete of thin cotton like.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831370A (en) * | 2016-03-22 | 2016-08-10 | 江南大学 | Preparation method of cocoa butter equivalent |
| CN105936922A (en) * | 2016-06-02 | 2016-09-14 | 北京化工大学 | Method for enzymatic transesterfication preparation of cocoa butter equiralent by using 33-DEG C palm oil |
| CN106035923A (en) * | 2016-06-12 | 2016-10-26 | 上海大学 | Method for preparing cocoa butter equivalent by aid of 28-degree palm oil medium fractionation substances (POMF) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100006A (en) * | 1985-04-01 | 1985-09-10 | 江西工业大学 | With oleum sapii (or seed) is the method that raw material is produced cocoa butter equivalent |
| CN101501203A (en) * | 2006-07-19 | 2009-08-05 | 日清奥利友集团株式会社 | Process for production of hard butter suitable for chocolate product |
| CN102869267A (en) * | 2010-04-22 | 2013-01-09 | Cj第一制糖株式会社 | Method of manufacturing hard butter similar to cacao butter |
-
2014
- 2014-12-26 CN CN201410823600.8A patent/CN104522264A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100006A (en) * | 1985-04-01 | 1985-09-10 | 江西工业大学 | With oleum sapii (or seed) is the method that raw material is produced cocoa butter equivalent |
| CN101501203A (en) * | 2006-07-19 | 2009-08-05 | 日清奥利友集团株式会社 | Process for production of hard butter suitable for chocolate product |
| CN102869267A (en) * | 2010-04-22 | 2013-01-09 | Cj第一制糖株式会社 | Method of manufacturing hard butter similar to cacao butter |
Non-Patent Citations (1)
| Title |
|---|
| 王海雄: "《上海大学硕士学位论文》", 31 December 2004 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105831370A (en) * | 2016-03-22 | 2016-08-10 | 江南大学 | Preparation method of cocoa butter equivalent |
| CN105831370B (en) * | 2016-03-22 | 2019-09-13 | 江南大学 | A method of preparing cacaolike butter |
| CN105936922A (en) * | 2016-06-02 | 2016-09-14 | 北京化工大学 | Method for enzymatic transesterfication preparation of cocoa butter equiralent by using 33-DEG C palm oil |
| CN105936922B (en) * | 2016-06-02 | 2020-03-17 | 北京化工大学 | Method for preparing cocoa butter equivalent by using palm oil enzymatic transesterification at 33 DEG C |
| CN106035923A (en) * | 2016-06-12 | 2016-10-26 | 上海大学 | Method for preparing cocoa butter equivalent by aid of 28-degree palm oil medium fractionation substances (POMF) |
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Inventor after: Weng Xinchu Inventor after: Li Cheng Inventor after: Song Yu Inventor before: Weng Xinchu Inventor before: Li Cheng Inventor before: Song Ning |
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