CN103627519A - Method for removing total cholesterol in animal fat - Google Patents
Method for removing total cholesterol in animal fat Download PDFInfo
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- CN103627519A CN103627519A CN201210312583.2A CN201210312583A CN103627519A CN 103627519 A CN103627519 A CN 103627519A CN 201210312583 A CN201210312583 A CN 201210312583A CN 103627519 A CN103627519 A CN 103627519A
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Abstract
The invention provides a method for removing total cholesterol in animal fat. The method comprises the following steps: first, esterification is performed, animal fat is subjected to an esterification reaction under action of catalysts; second, adsorption is performed, the products after esterification reaction are contacted with adsorbents; third, the products after adsorption reaction is subjected to solid-liquid separation. In the method, no extra reaction substrates need to be added, no superfluous reactants need to be removed in the subsequent separating and processing steps, and the operation is simple. The polarity of the products after esterification weakens, and the products are easy to be absorbed by the adsorbents. The removing rates of free cholesterol and total cholesterol through the esterification and adsorption two-step method are both higher than that only through an adsorption method.
Description
Technical field
The present invention relates to the complete processing of animal tallow, is a kind of improved animal tallow complete processing specifically, more particularly, the present invention relates to a kind of method of removing cholesterol in animal tallow.
Background technology
Cholesterol in animal grease with dissociate and two kinds of forms of combined exist, the cholesterol of combined be hydroxyl by Esterification of Free Fat Acid cholesteryl ester, as cholesterol acid ester or cholesterol cetylate etc.In butterfat, generally contain the cholesterol of 0.25%-0.3%, in butter, the general content of cholesterol is 0.1%-0.2%, and in yolk, content is higher, accounts for greatly the 0.5%-2.5% of dry weight.
As everyone knows, very high serum cholesterol content, hypertension, abnormal electrocardiographic pattern etc. are all the important factors that causes heart attack.Much research in recent years finds that high-content plasma cholesterol can cause atherosclerosis, and risk of coronary heart disease is strengthened.In human body, high-content serum cholesterol major cause has the familial hypercholesterolemia of heredity confusion, heterozygosis and often eats high saturated fatty-calorie-cholesterol diet.Nutrition and fitness guru think that the cholesterol level in keeping on a diet is that prevention and the first step for the treatment of hypercholesterolemia and hyperlipoidemia disease are also important steps simultaneously.Therefore, in research reduction food, cholesterol level especially reduces cholesterol level in animal tallow and causes many investigators' interest.
CN101292020 discloses a kind of method that adopts sterol in sorbent material absorb oil, and wherein said sorbent material comprises clay, silicon-dioxide or their mixture.Sterol is wherein the material that a class comprises cholesterol (free cholesterol and cholesteryl ester) and plant sterol.
US5128162 (A) adopts sweet three ester oils and polynary acylting agent generation esterification containing cholesterol; obtain the mixture that polarity becomes sweet three ester oils of large cholesteryl monoesters, unreacted polynary acyl group reagent and cholesterol; then separated unreacted polynary acyl group reagent; remaining mixture is reacted with parting material; reclaim sweet three ester oils, obtained removing sweet three ester oils of cholesterol.In this method, polynary acylting agent, as the reactant of esterification, comprises cyclic acid anhydride and polyprotonic acid halogenide etc., and free acid is as the catalyzer of this reaction.The shortcoming of this method: (1) reactant system is complicated, needs the extra reactant that adds.(2) complex operation step; because it is large that esterification after product polarity becomes; the modes such as alkaline aqueous solution or anionite-exchange resin of need to adding are removed, and unnecessary polynary acylting agent also needs washing or centrifugal or solvent extraction to remove in addition, and industrialization is can operational degree low.
Therefore, be necessary to provide a kind of new method that removes total cholesterol in grease, to overcome now methodical above-mentioned defect, significantly improve removing cholesterol rate.
Summary of the invention
To this, contriver has done a large amount of further investigation work, propose a kind of new method that removes total cholesterol in grease, especially removed the method for total cholesterol in animal tallow, adopted the removing cholesterol rate of the method to increase significantly compared with prior art removing cholesterol rate.
The object of the invention is to provide a kind of method that removes cholesterol in animal tallow.
Provided by the inventionly remove the method for cholesterol in animal tallow and comprise the following steps:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs, obtains esterification products;
(2) absorption: esterification reaction product is contacted with sorbent material, obtain adsorbed product;
(3) separation: adsorbed product is carried out to solid-liquid separation.
In a preference, described in be separated into that centrifugation, natural subsidence are separated, separatory is separated or filtering separation.
In another preference, esterification comprises chemical method esterification, enzyme process esterification.
In another preference, chemical method esterification reaction temperature is 130 ~ 250 ℃, and enzyme process esterification temperature is 20 ~ 110 ℃.
In another preference, in chemical method esterification process, animal tallow is contacted with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 130 ~ 250 ℃, or after contact forms mixture, regulates temperature to 130 ~ 250 ℃ of described mixture.
In another preference, chemical catalyst for esterification reaction is one or more in aluminum oxide, aluminium hydroxide, silicon-dioxide, Vanadium Pentoxide in FLAKES, phosphoric acid etc.
In another preference, chemical catalyst for esterification reaction consumption is 0.01% ~ 2% of animal tallow weight, preferably 0.3% ~ 1%.
In another preference, chemical reaction time of esterification is 0.5 ~ 12h.
In another preference, in enzyme process esterification process, animal tallow is contacted with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 20 ~ 110 ℃, or after contact forms mixture, regulates temperature to 20 ~ 110 ℃ of described mixture.
In another preference, enzyme process catalyst for esterification reaction is one or more in lipase, Esterified Enzyme.
In another preference, enzyme process catalyst for esterification reaction consumption is 0.1% ~ 20% of animal tallow weight.
In another preference, enzyme process reaction time of esterification is 0.5 ~ 24h.
In another preference, absorption reaction temperature is 100-200 ℃.
In another preference, sorption reaction time is 1 ~ 120min.
In another preference, sorbent material is one or more in carclazyte, gac, silicon-dioxide, Trisyl.
In another preference, sorbent material consumption is 0.5% ~ 10% of animal tallow weight, preferably 2% ~ 10%.
In another preference, in described animal tallow, contained free fatty acids is more than or equal to 0.5:1 with the mol ratio of contained free cholesterol wherein.
In another preference, described animal tallow is selected from one or more in fish oil, lard, butter, chicken fat, duck fat, butterfat, and preferably animal tallow is selected from fish oil, lard, butter or its combination.
In adopting some preferred embodiment of preceding method, also be included in before absorption reaction and also comprise esterification reaction product is carried out to separated for the first time step, preferably, separation for the first time can be for centrifugation, natural subsidence separation, separatory is separated or filtering separation.
Nutritionist advises that the cholesterol intake of per day for adults should be lower than 300mg, to cardiovascular patient, and should be lower than 200mg.Especially 2008 Nian， Ministry of Health notices are printed and distributed in < < Food Nutrition Labeling management regulation > > the content requirement of cholesterol are limited.So, remove or the cholesterol level that reduces in hypercholesterolemia food is that market is required.
Therefore, a further object of the invention is to provide a kind of animal tallow.
Animal tallow provided by the invention is to remove according to above-mentioned the animal tallow that in animal tallow prepared by the method for total cholesterol.
A further object of the invention is to provide the purposes of this animal tallow.
Animal fat of the present invention is for the preparation of food or medicine.
Method of the present invention has the following advantages:
(1) the inventive method is without adding extra reaction substrate, without removing unnecessary reactant, simple to operate in later separation treatment step;
(2) the esterification absorption two-step approach that the present invention adopts to the decreasing ratio of free cholesterol and total cholesterol all higher than the adsorption effect that only adopts absorption method.
Embodiment
" scope " disclosed herein is with the form of lower limit and the upper limit.Can be respectively one or more lower limits, and one or more upper limit.Given range limits by a selected lower limit and a upper limit.Selected lower limit and the upper limit define the border of special scope.All scopes that can limit by this way comprise with capable of being combined, and any lower limit can be combined to form a scope with any upper limit.For example, for special parameter, listed the scope of 60-120 and 80-110, be interpreted as that the scope of 60-110 and 80-120 also expects.In addition, if the minimum extent value 1 and 2 of listing, and if listed maximum range value 3,4 and 5, scope below can all expect: 1-3,1-4,1-5,2-3,2-4 and 2-5.
In the present invention, unless have other explanation, the content range of each component of composition with and preferable range between can mutually be combined to form new technical scheme.
In the present invention, unless there are other explanations, " its combination " represents the multicomponent mixture of described each element, for example two kinds, three kinds, four kinds and until the multicomponent mixture of maximum possible.
In the present invention, unless there are other explanations, all " part " and percentage ratio (%) all refer to weight percentage.
In the present invention, unless there are other explanations, in all compositions, the percentage ratio sum of each component is 100%.
In the present invention, unless there are other explanations, numerical range " a-b " represents that the breviary that a closes to the arbitrary real array between b represents, wherein a and b are real numbers.For example numerical range " 0-5 " represents all to have listed the whole real numbers between " 0-5 " herein, and " 0-5 " just the breviary of these combinations of values represents.
If do not particularly not pointed out, this specification sheets term " a kind of " used refers to " at least one ".
If do not particularly not pointed out, the benchmark of percentage ratio of the present invention (comprising weight percentage) is all the gross weight of described composition.
In this article, except as otherwise noted, the ratio of each component or weight all refer to dry weight.
In the present invention, if not special explanation, all embodiments mentioned in this article and preferred implementation can be combined to form new technical scheme mutually.
In the present invention, if not special explanation, all technical characterictics mentioned in this article and preferred feature can be combined to form new technical scheme mutually.
In the present invention, if not special explanation mentioned in this article can sequentially be carried out in steps, also can carry out at random, but preferably in sequence.For example, described method comprises step (a) and (b), represents that described method can comprise in sequence step (a) and (b), also can comprise in sequence step (b) and (a).For example, describedly mention described method and also can comprise step (c), represent that step (c) can random order join described method, for example, described method can comprise step (a) and (b) and (c), also step (a), (c) and (b) be can comprise, step (c), (a) and (b) etc. also can be comprised.
In the present invention, if not special explanation, " comprising " mentioned in this article represents open, can be also closed.For example, described " comprising " can represent to comprise other elements of not listing, also can only comprise the element of listing.
In the present invention, if there is no special explanation, the concrete numerical value in embodiment and concrete material can be combined with other features of description part herein herein.For example, the temperature that description part is herein mentioned reaction is 10-100 ℃, and the temperature of reaction that embodiment mentions is 20 ℃, can think so and specifically disclose the scope of 10-20 ℃ herein, or the scope of 20-100 ℃, and this scope other features that can describe part combine and form new technical scheme.Again for example, describe part herein and mention a compounds alcohol, and the concrete alcohol that embodiment mentions is ethanol, ethanol can combine and form new technical scheme with other feature of describing part so.
Method
The invention provides a kind of method that removes cholesterol in grease, said method comprising the steps of:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs, obtains esterification reaction product;
(2) absorption: esterification reaction product is contacted with sorbent material, obtain adsorbed product;
(3) separation: adsorbed product is carried out to solid-liquid separation.
In the present invention, term " separation " refers to the method or the process that are divided into separated two-phase (as solid phase and liquid phase) of the mixture (as esterification reaction product and/or or adsorbed product) obtaining.To those skilled in the art, for reaching separated object, adoptable separation method is conventional, those of ordinary skill in the art also can directly determine in conjunction with prior art according to description of the invention again, for example, include but not limited to utilize material the aspects such as density difference or utilize material granular size difference or utilize the difference etc. of the permeability of material to carry out separation, particularly, adoptable separation method includes but not limited to centrifugation in the present invention, natural subsidence is separated, separatory separation or filtering separation, in these methods, different and the difference to some extent of the concrete parameter vision method using, but to those skilled in the art, all conventional, those of ordinary skill in the art also can directly determine in conjunction with prior art according to description of the invention again.
In the present invention, if not special explanation, " animal tallow " as herein described or " animal fat " refer to such an extent that be fat or the grease that derives from animal and contain cholesterol, particularly, include but not limited to fish oil, lard, butter, chicken and duck fat, butterfat or its combination.
In the present invention, if not special explanation, " cholesterol " as herein described is a kind of derivative of perhydrocyclopentanophenanthrene, it is present in lipoprotein in blood, and its existence form comprises that high density lipoprotein cholesterol, low density lipoprotein cholesterol, extra-low density protein cholesterol are several.In animal tallow, also having cholesterol, there is impact to the quality of animal grease in its content.
In the present invention, if not special explanation, " free cholesterol " as herein described refers to the cholesterol existing with free state form, the cholesterol particularly existing with free state form in animal grease.
In the present invention, if not special explanation, " combined cholesterol " as herein described refers to the cholesteryl ester of being combined with lipid acid, the cholesteryl ester of being particularly combined with lipid acid in animal grease.
In the present invention, if not special explanation, " total cholesterol " as herein described refers to the general designation of free state cholesterol and combined cholesterol.
In the present invention, esterification refers to alcohol and with carboxylic acid or oxygen-containing inorganic acid, generates the reaction of ester and water, esterification need to add catalyzer with accelerated reaction conventionally, and according to the difference of the catalyzer using, esterification can comprise chemical method esterification, enzyme process esterification etc.
In the present invention, if there is no special explanation, chemical method esterification as herein described refers to that alcohol follows carboxylic acid or oxygen-containing inorganic acid under the effect of chemical catalyst, to generate the reaction of ester and water.In the present invention, " chemical catalyst " refers to and presents its natural form or be rendered as the catalyst substance with the form of mixtures of the carrier of preparing according to technology well known by persons skilled in the art or matrix." chemical catalyst " that in esterification, use is well known to those skilled in the art, and can include but not limited to for the chemical catalyst of esterification an acidic catalyst, basic catalyst etc.Particularly, include but not limited to one or more in aluminum oxide, aluminium hydroxide, silicon-dioxide, Vanadium Pentoxide in FLAKES, phosphoric acid etc.Preferably, the aluminum oxide of use is including, but not limited to α-Al
2o
3, β-Al
2o
3, γ-Al
2o
3deng or its their mixture or composition.Those skilled in the art can also, according to instruction of the present invention, use other chemical catalysts of reporting in existing document.
In the present invention, if there is no special explanation, enzyme process esterification as herein described refers to that alcohol follows carboxylic acid or oxygen-containing inorganic acid under the katalysis of specific biological enzyme, to generate the reaction of ester and water, the enzyme that can be used for the esterification of catalysis enzyme process is conventional for a person skilled in the art, comprise the various enzymes that can be used for catalytic esterification, for example can lipase, one or more in Esterified Enzyme, particularly, can include but not limited to Lipozyme 435, Lipozyme RMIM, Lipozyme TLIM.
In another preference, chemical method esterification reaction temperature is 130 ~ 250 ℃, and enzyme process esterification temperature is 20 ~ 110 ℃.
In another preference, in chemical method esterification process, animal tallow is contacted with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 130 ~ 250 ℃, or after contact forms mixture, regulates temperature to 130 ~ 250 ℃ of described mixture.
In another preference, in enzyme process esterification process, animal tallow is contacted with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 20 ~ 110 ℃, or after contact forms mixture, regulates temperature to 20 ~ 110 ℃ of described mixture.
In the present invention, enzyme as herein described is including, but not limited to Rhizopus, Aspergillus, Mucor, bacterium, yeast.
In another preference, enzyme process catalyst for esterification reaction consumption is 0.1% ~ 20% of animal tallow weight.
In another preference, enzyme process reaction time of esterification is 0.5 ~ 24h.
In the present invention, " absorption " refer to material (being mainly solid matter) surface and hold a certain component in surrounding medium (liquid or gas) or the phenomenon of some component.To those skilled in the art, in liquid (as grease), add sorbent material (normally thering is adsorbing solid matter), so that the specific components in this liquid (particularly impurity) is removed maybe by the target components enrichment in this liquid, be a kind of routine techniques means.In the present invention, " sorbent material " be any can be by another kind of material being adsorbed onto to its lip-deep solid-state and fixing material with molecules of interest direct interaction or with being attached to the Compound Phase mutual effect on sorbent material.To those skilled in the art, for reaching the object of absorption, adoptable method is conventional, and those of ordinary skill in the art also can directly determine in conjunction with prior art according to description of the invention again.For example, the sorbent material of use is being known in the art and can easily obtaining by commercial sources, for example, can be one or more in carclazyte, gac, silicon-dioxide, Trisyl.While using sorbent material to adsorb, the amounts of the sorbent material of the adsorption temp adopting, the adsorption time that absorption reaction is carried out, use etc. to those skilled in the art, are conventional, or on the basis of content disclosed by the invention, in conjunction with prior art, directly determine.
In the present invention, spendable silicon-dioxide is including, but not limited to silica, precipitated silica, fumed silica, silica gel, soft silica and composition thereof etc.; " carclazyte " refers to that with clay (being mainly wilkinite) be raw material, through mineral acid treatment, then through water rinse, the dry sorbent material of making, but spendable carclazyte includes but not limited to use aforesaid method to obtain in the present invention; " Trisyl " as herein described is a kind of silica gel hydrogel.But scope of the present invention is not limited to this.
In a preference of the present invention, the temperature of described absorption reaction is 100-200 ℃, 110-200 ℃ preferably, 120-200 ℃, 130-200 ℃, 140-200 ℃, 150-200 ℃, 160-200 ℃, 170-200 ℃, 180-200 ℃, 190-200 ℃, 100-190 ℃, 110-190 ℃, 120-190 ℃, 130-190 ℃, 140-190 ℃, 150-190 ℃, 160-190 ℃, 170-190 ℃, 180-190 ℃, 100-180 ℃, 110-180 ℃, 120-180 ℃, 130-180 ℃, 140-180 ℃, 150-180 ℃, 160-180 ℃, 170-180 ℃, 100-170 ℃, 110-170 ℃, 120-170 ℃, 130-170 ℃, 140-170 ℃, 150-170 ℃, 160-170 ℃, 100-160 ℃, 110-160 ℃, 120-160 ℃, 130-160 ℃, 140-160 ℃, 150-160 ℃, 100-150 ℃, 110-150 ℃, 120-150 ℃, 130-150 ℃, 140-150 ℃, 100-140 ℃, 110-140 ℃, 120-140 ℃, 130-140 ℃, 100-130 ℃, 110-130 ℃, 120-130 ℃, 100-120 ℃, 110-120 ℃, 100-110 ℃.
In a preference of the present invention, the time of described absorption reaction is 1 ~ 120min, be preferably 10 ~ 120min, 20 ~ 120min, 30 ~ 120min, 40 ~ 120min, 50 ~ 120min, 60 ~ 120min, 70 ~ 120min, 80 ~ 120min, 90 ~ 120min, 100 ~ 120min, 110 ~ 120min, 10 ~ 110min, 20 ~ 110min, 30 ~ 110min, 40 ~ 110min, 50 ~ 110min, 60 ~ 110min, 70 ~ 110min, 80 ~ 110min, 90 ~ 110min, 100 ~ 110min, 10 ~ 100min, 20 ~ 100min, 30 ~ 100min, 40 ~ 100min, 50 ~ 100min, 60 ~ 100min, 70 ~ 100min, 80 ~ 100min, 90 ~ 100min, 10 ~ 90min, 20 ~ 90min, 30 ~ 90min, 40 ~ 90min, 50 ~ 90min, 60 ~ 90min, 70 ~ 90min, 80 ~ 90min, 10 ~ 80min, 20 ~ 80min, 30 ~ 80min, 40 ~ 80min, 50 ~ 80min, 60 ~ 80min, 70 ~ 80min, 10 ~ 70min, 20 ~ 70min, 30 ~ 70min, 40 ~ 70min, 50 ~ 70min, 60 ~ 70min, 10 ~ 60min, 20 ~ 60min, 30 ~ 60min, 40 ~ 60min, 50 ~ 60min, 10 ~ 50min, 20 ~ 50min, 30 ~ 50min, 40 ~ 50min, 10 ~ 40min, 20 ~ 40min, 30 ~ 40min, 10 ~ 30min, 20 ~ 30min, 10 ~ 20min.
In a preference of the present invention, sorbent material consumption is 0.5% ~ 10% of animal tallow weight (W/W), preferably 1% ~ 10%, and 2% ~ 10%, 2%-9%, 3%-8%, 4%-8%, 5%-7%, 5%-6%, 6%-7%, 2%-5%, 3%-7%.
In another preference, in described animal tallow, contained free fatty acids is more than or equal to 0.5:1 with the mol ratio of contained free cholesterol wherein.
In another preference, described animal tallow wide material sources, it can be for example the grease that includes but not limited to one or more sources in fish, bird and/or beasts, preferably, include but not limited to be selected from one or more in fish oil, lard, butter, chicken fat, duck fat, butterfat, more preferably animal tallow is selected from fish oil, lard, butter or its combination.
In the present invention, described animal fat is selected from fish oil, lard, butter, chicken and duck fat, butterfat or its combination; Preferably, described animal fat is selected from fish oil, lard, butter or its combination.Fish oil can be oil separated from fish, including, but not limited to grass carp oil, carp is oily, crucian is oily, seal oil, shark oil shai, cittle fish oil, octopus oil, dab oil, sardine oil, perch oil, whale oil, salmon oil, cod oil, mullet are oily, bonito oil etc., comprises their mixture and composition.
In adopting some preferred embodiments of preceding method, before absorption reaction, also comprise the step of esterification reaction product being carried out to separation (separated for the first time, being separated into after corresponding absorption reaction " separation " or " separated for the second time ").
To those skilled in the art, for reaching separated object, in " separated for the first time " step, adoptable separation method can be conventional, those of ordinary skill in the art also can directly determine in conjunction with prior art according to description of the invention again, for example, include but not limited to utilize material the aspects such as density difference or utilize material granular size difference or utilize the difference etc. of the permeability of material to carry out separation, particularly, in " separated for the first time " of the present invention step, adoptable separation method includes but not limited to centrifugation, natural subsidence is separated, separatory separation or filtering separation, in these methods, different and the difference to some extent of the concrete parameter vision method using, but to those skilled in the art, all conventional, those of ordinary skill in the art also can directly determine in conjunction with prior art according to description of the invention again.
Product and purposes
The present invention also provides and has used the animal fat of animal tallow prepared by method of the present invention and preparation for the preparation of the purposes of food or medicine.
Beneficial effect
Method of the present invention has the following advantages:
(1) the inventive method is without adding extra reaction substrate, without removing unnecessary reactant, simple to operate in later separation treatment step;
(2) the esterification absorption two-step approach that the present invention adopts to the decreasing ratio of free cholesterol and total cholesterol all higher than the adsorption effect that only adopts absorption method.
In the present invention, for accelerating the speed of response of esterif iotacation step, stirring is an optional method.The method of described stirring is conventional, those of ordinary skill in the art can directly determine in conjunction with prior art the concrete constant stirring again according to description of the invention, so that the free fatty acids in animal tallow fully reacts under the effect of catalyzer with free cholesterol.In a preference of the present invention, the rotating speed of described stirring is 1 ~ 500 rev/min, preferably 10 ~ 200 revs/min, more preferably 20 ~ 100 revs/min, is preferably 40 ~ 80 revs/min.
As no specific instructions, various raw material of the present invention all can obtain by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or described herein, the familiar same meaning of all specialties used herein and scientific words and those skilled in the art.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
Below in conjunction with embodiment, describe the present invention in detail, but scope of the present invention is not limited to this.
Raw material
Trisyl: purchased from Grace company;
SiO
2: purchased from Chemical Reagent Co., Ltd., Sinopharm Group;
Active A l
2o
3: purchased from Aladdin reagent (Shanghai) Co., Ltd.;
Atlapulgite: purchased from Mt. Huang in Anhui Tai Ke activated Fuller earth company limited;
The enzyme using: purchased from Novozymes Company;
Fish oil: purchased from Peru TASA company;
Lard, butter, butterfat are all purchased from Southseas Specialty Fats Industrial (Shanghai) Co., Ltd.;
The buying of chicken and duck fat is from Nong Pi market, the Five continents, Shanghai City.
Detection method
Total cholesterol detects: GB/T9695.24-2008 meat and meat product Determination of Cholesterol Content.
The detection of free cholesterol: the mensuration of GB/T25223-2010 animal-plant oil sterol composition and sterol total amount
Plant and instrument
Gas chromatograph, Agilent6890, purchased from Agilent; Detector: flame ionization detector, FID.
Comparative example 1:
Animal grease is heated to 100 ~ 200 ℃, adds sorbent material, under vacuum condition, react 1 ~ 120min.Reaction finishes rear centrifugal its solid-liquid separation that makes, and gets liquid phase, has obtained removing the animal grease of part free cholesterol and total cholesterol.
The experiment condition of comparative example 1 each experiment and experimental result are in Table 1.
Table 1: the experiment condition of comparative example 1 and experimental result
Comparative example 2:
By animal grease heating, add 1% (weight) SiO
2make catalyzer, vacuum tightness 5mbar, carries out esterification 1h at 180 ℃.Centrifugal its solid-liquid separation that makes, gets liquid phase.Then adopt other cholesterol reduction methods of reporting (extracting the technical study. Hu Wenna of cholesterol from lanosterol, Zhejiang University's master thesis [D], 2011.) to remove total cholesterol.Concrete grammar is as follows: gets the oil phase after above-mentioned separation, under normal temperature, adds the dehydrated alcohol that volume ratio is 1:1, and extraction 10min, standing separatory, gets upper oil phase and continues to add the dehydrated alcohol that volume ratio is 1:1, repeats aforesaid operations 3 times.Get oil phase rotary evaporation, remove residual dehydrated alcohol, detect the total cholesterol level in the oil phase after rotary evaporation.
After above-mentioned first esterification, extract in contrast the method that removes cholesterol, only adopt the extraction of dehydrated alcohol method.Get animal grease, under normal temperature, add the dehydrated alcohol that volume ratio is 1:1, extraction 10min, standing separatory, gets upper oil phase and continues to add the dehydrated alcohol that volume ratio is 1:1, repeats aforesaid operations 3 times.Get oil phase rotary evaporation, remove residual dehydrated alcohol, detect the total cholesterol level of the oil phase after evaporation.Under this condition, the total cholesterol decreasing ratio of fish oil, lard and butter is respectively 34%, 40%, 37%.
The experiment condition of comparative example 2 and experimental result are in Table 2.
Table 2: the experiment condition of comparative example 2 and experimental result
As can be seen from Table 2, adopt the total cholesterol decreasing ratio of the method for extraction treatment after first esterification identical with the total cholesterol decreasing ratio of direct extraction treatment.Be that esterification is not effective Pretreatment to other cholesterol reduction methods beyond absorption method, can not increase the effect of follow-up cholesterol reduction.
Embodiment 1:
Chemical method esterification+absorption
By animal grease heating, add catalyst for esterification reaction, at a certain temperature, vacuum keep 10mbar carries out esterification for some time below.After this reaction system has been reacted, the centrifugal solid-liquid separation that makes, gets liquid phase; Then above-mentioned animal grease is heated to 100～200 ℃, adds sorbent material, under vacuum condition, react 1～120 minute.After this reaction system reaction finishes, suction filtration makes solid-liquid separation, obtains the animal grease of low total cholesterol and low free cholesterol.The experiment condition of embodiment 1 is in Table 3.
The experiment condition of table 3: embodiment 1
In embodiment 1, each experimental result contrasts in Table 4 with comparative example 1 result.
Table 4: embodiment 1 each experimental result contrasts with comparative example 1 experimental result
By table 4 result, can be found out, adopt the present invention's chemistry esterification and absorption two-step approach to the decreasing ratio of the total cholesterol of grease and free cholesterol all higher than a step absorption method, and high energy improves more than 10 times.
Embodiment 2
Enzyme process esterification+absorption
By animal grease heating, add enzyme process catalyst for esterification reaction, at a certain temperature, vacuum keep 10mbar carries out esterification for some time below.After this reaction system has been reacted, the centrifugal solid-liquid separation that makes, gets liquid phase; Then resulting liquid phase in previous step is heated to 100～200 ℃, adds sorbent material, under vacuum condition, react 1～120 minute.After this reaction system reaction finishes, suction filtration makes solid-liquid separation, obtains the animal grease of low total cholesterol and low free cholesterol.The experiment condition of embodiment 2 is in Table 5.
The experiment condition of table 5 embodiment 2
In embodiment 2, each experimental result contrasts in Table 6 with comparative example 1 result.
Table 6: embodiment 2 each experimental results contrast with comparative example 1 experimental result
By table 6 result, can be found out, adopt enzyme process esterification of the present invention and absorption two-step approach to the decreasing ratio of the total cholesterol of grease and free cholesterol all higher than a step absorption method.
Embodiment 3
In preceding method, for avoiding the impact on absorption, after esterification, carried out separation.For investigating the impact of this step, contriver processes corresponding grease by the method for embodiment 1 and 2 respectively again, but after esterification, directly use esterification products to carry out adsorption operations, rather than use the liquid product that carries out in advance solid-liquid separation acquisition to adsorb, detect respectively the decreasing ratio of free cholesterol and total cholesterol, and the grease of processing with method by embodiment 1 and 2 and comparing with the free cholesterol of grease and the decreasing ratio of total cholesterol that existing method is processed.
Experimental result shows, adopts the method for embodiment 3 to use esterification products directly to adsorb, and the decreasing ratio of its total cholesterol and free cholesterol is a little less than the decreasing ratio that adopts the correlation method of embodiment 1 and 2.But adopt the method for embodiment 3 to process grease, the decreasing ratio of its total cholesterol and free cholesterol is the decreasing ratio of total cholesterol and free cholesterol when adopting a step absorption method still, even find, in a best result, removing cholesterol rate has improved 8 times.
The foregoing is only preferred embodiment of the present invention, not in order to limit essence technology contents scope of the present invention, essence technology contents of the present invention is to be broadly defined in the claim scope of application, any technology entity or method that other people complete, if defined identical with the claim scope of application, also or a kind of change of equivalence, all will be regarded as being covered by among this claim scope.
All documents of mentioning in the present invention are all quoted as a reference in this application, just as each piece of document, are quoted as a reference separately.In addition should be understood that, after having read foregoing of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (25)
1. a method that removes total cholesterol in animal tallow, said method comprising the steps of:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs, obtains esterification reaction product;
(2) absorption: esterification reaction product contacts with sorbent material, obtains adsorbed product;
(3) separation: adsorbed product is carried out to solid-liquid separation.
2. the method for claim 1, is characterized in that, described in be separated into that centrifugation, natural subsidence are separated, separatory is separated or filtering separation.
3. the method for claim 1, is characterized in that, described contact is for to join described sorbent material in described esterification reaction product.
4. the method for claim 1, is characterized in that, before described contact, regulates esterification reaction product temperature, or at esterification reaction product, contacts the temperature that regulates described mixture after formation mixture with sorbent material.
5. the method for claim 1, is characterized in that, described esterification comprises chemical method esterification, enzyme process esterification.
6. method as claimed in claim 5, is characterized in that, in chemical method esterification process, animal tallow is contacted with esterifying catalyst.
7. method as claimed in claim 6, is characterized in that, before contact, described animal tallow temperature is adjusted to 130 ~ 250 ℃, or regulates described mixture temperature to 130 ~ 250 ℃ after the two contact forms mixture.
8. method as claimed in claim 6, is characterized in that, described esterifying catalyst is one or more in aluminum oxide, Vanadium Pentoxide in FLAKES, aluminium hydroxide, phosphoric acid, silicon-dioxide.
9. method as claimed in claim 8, is characterized in that, esterifying catalyst consumption is 0.01% ~ 2% of described animal tallow weight, preferably 0.3% ~ 1%.
10. method as claimed in claim 5, is characterized in that, chemical method reaction time of esterification is 0.5 ~ 12h.
11. methods as claimed in claim 5, is characterized in that, in enzyme process esterification process, animal tallow are contacted with esterifying catalyst.
12. methods as claimed in claim 11, is characterized in that, before contact, described animal tallow temperature are adjusted to 20 ~ 110 ℃, or after the two contact forms mixture, regulate temperature to 20 ~ 110 ℃ of described mixture.
13. methods as claimed in claim 11, is characterized in that, described esterifying catalyst is one or more in lipase, Esterified Enzyme.
14. methods as claimed in claim 11, is characterized in that, described esterifying catalyst consumption is 0.1% ~ 20% of animal tallow weight.
15. methods as claimed in claim 11, is characterized in that, the reaction times of described enzyme process esterification is 0.5 ~ 24h.
16. the method for claim 1, is characterized in that, the adsorption temp of step (3) is 100 ~ 200 ℃.
17. the method for claim 1, is characterized in that, the adsorption time of step (3) is 1 ~ 120min.
18. the method for claim 1, is characterized in that, described sorbent material is one or more in carclazyte, gac, silicon-dioxide, Trisyl.
19. the method for claim 1, is characterized in that, the consumption of described sorbent material is 0.5% ~ 10% of animal tallow weight, preferably 2% ~ 10%.
20. the method for claim 1, is characterized in that, in described animal tallow, the mol ratio of the contained free fatty acids free cholesterol contained with it is more than or equal to 0.5:1.
21. methods as claimed in claim 20, is characterized in that, described animal tallow is selected from fish oil, lard, butter, chicken and duck fat, butterfat or its combination; Preferably, described animal tallow is selected from fish oil, lard, butter or its combination.
22. methods as described in any one in claim 1-21, is characterized in that, also comprise esterification reaction product is carried out to separated for the first time step, to obtain liquid phase before absorption reaction.
23. methods as claimed in claim 22, is characterized in that, are describedly separated into for the first time that centrifugation, natural subsidence are separated, separatory is separated or filtering separation.
Animal tallow prepared by 24. methods as described in any one in claim 1-23.
25. animal fats as claimed in claim 24 are for the preparation of the purposes of food or medicine.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446124A (en) * | 2017-07-26 | 2017-12-08 | 浙江皇马科技股份有限公司 | The preparation method of fatty alcohol phosphate polyethenoxy ether |
| CN113046166A (en) * | 2019-12-26 | 2021-06-29 | 丰益(上海)生物技术研发中心有限公司 | Oil and fat composition |
| CN113115833A (en) * | 2019-12-31 | 2021-07-16 | 丰益(上海)生物技术研发中心有限公司 | Thick soup and preparation process thereof |
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| CN113287737A (en) * | 2021-06-09 | 2021-08-24 | 四川航佳生物科技有限公司 | Chafing dish beef tallow and preparation method thereof |
| CN113438948A (en) * | 2018-12-06 | 2021-09-24 | 艾帕克斯挪威联合股份有限公司 | Very long chain fatty acid compositions |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2218989A (en) * | 1987-12-15 | 1989-11-29 | Inst Penyelidikan Minyak Kelap | Recovery of carotenoids, tocopherols, tocotrienols and sterols from esterified palm oil |
| US5128162A (en) * | 1990-07-31 | 1992-07-07 | Kraft General Foods, Inc. | Method for removing cholesterol from edible oils |
| CN1334703A (en) * | 1998-12-10 | 2002-02-06 | 阿兹·查菲克·阿瓦德 | Method to reduce free fatty acids and cholesterol in anhydrous animal fat |
| JP2003160795A (en) * | 2001-11-27 | 2003-06-06 | Asahi Denka Kogyo Kk | Method for producing phytosterol/fatty acid ester- containing oil-and-fat composition |
| CN1958596A (en) * | 2006-11-22 | 2007-05-09 | 浙江大学 | Method for extracting cholesterol from lanoline |
| CN101292020A (en) * | 2005-08-26 | 2008-10-22 | 加拿大海洋营养食品有限公司 | A process for the removal of sterols and other compounds from glycerol oils |
| CN102190700A (en) * | 2010-03-12 | 2011-09-21 | 丰益(上海)生物技术研发中心有限公司 | Method for preparing fatty acid phytosterol esters |
-
2012
- 2012-08-29 CN CN201210312583.2A patent/CN103627519B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2218989A (en) * | 1987-12-15 | 1989-11-29 | Inst Penyelidikan Minyak Kelap | Recovery of carotenoids, tocopherols, tocotrienols and sterols from esterified palm oil |
| US5128162A (en) * | 1990-07-31 | 1992-07-07 | Kraft General Foods, Inc. | Method for removing cholesterol from edible oils |
| CN1334703A (en) * | 1998-12-10 | 2002-02-06 | 阿兹·查菲克·阿瓦德 | Method to reduce free fatty acids and cholesterol in anhydrous animal fat |
| JP2003160795A (en) * | 2001-11-27 | 2003-06-06 | Asahi Denka Kogyo Kk | Method for producing phytosterol/fatty acid ester- containing oil-and-fat composition |
| CN101292020A (en) * | 2005-08-26 | 2008-10-22 | 加拿大海洋营养食品有限公司 | A process for the removal of sterols and other compounds from glycerol oils |
| CN1958596A (en) * | 2006-11-22 | 2007-05-09 | 浙江大学 | Method for extracting cholesterol from lanoline |
| CN102190700A (en) * | 2010-03-12 | 2011-09-21 | 丰益(上海)生物技术研发中心有限公司 | Method for preparing fatty acid phytosterol esters |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107446124A (en) * | 2017-07-26 | 2017-12-08 | 浙江皇马科技股份有限公司 | The preparation method of fatty alcohol phosphate polyethenoxy ether |
| CN113438948A (en) * | 2018-12-06 | 2021-09-24 | 艾帕克斯挪威联合股份有限公司 | Very long chain fatty acid compositions |
| CN113046166A (en) * | 2019-12-26 | 2021-06-29 | 丰益(上海)生物技术研发中心有限公司 | Oil and fat composition |
| CN113115833A (en) * | 2019-12-31 | 2021-07-16 | 丰益(上海)生物技术研发中心有限公司 | Thick soup and preparation process thereof |
| CN113293057A (en) * | 2021-04-23 | 2021-08-24 | 洛阳师范学院 | In-situ low-temperature ball milling leaching method for peony seed oil |
| CN113293057B (en) * | 2021-04-23 | 2022-09-30 | 洛阳师范学院 | In-situ low-temperature ball milling leaching method for peony seed oil |
| CN113287737A (en) * | 2021-06-09 | 2021-08-24 | 四川航佳生物科技有限公司 | Chafing dish beef tallow and preparation method thereof |
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|---|---|
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