CN103627519B - A kind of de-method except total cholesterol in animal tallow - Google Patents
A kind of de-method except total cholesterol in animal tallow Download PDFInfo
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- CN103627519B CN103627519B CN201210312583.2A CN201210312583A CN103627519B CN 103627519 B CN103627519 B CN 103627519B CN 201210312583 A CN201210312583 A CN 201210312583A CN 103627519 B CN103627519 B CN 103627519B
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Abstract
The present invention provides a kind of de-method except total cholesterol in animal tallow, and described method comprises the following steps: (1) esterification: animal grease, under the effect of catalyzer, esterification occurs; (2) adsorb: by the product of esterification and adsorbent contact; And the product after absorption reaction is carried out solid-liquid separation by (3). Adopt the inventive method without the need to adding extra reaction substrate, without the need to removing unnecessary reactant in later separation treatment step, simple to operate; Esterification after product polarity becomes weak, more easily by adsorbent; Esterification absorption two-step approach to the decreasing ratio of free cholesterol and total cholesterol all higher than the adsorption effect only adopting absorption method.
Description
Technical field
The present invention relates to the complete processing of animal tallow, it is the animal tallow complete processing of a kind of improvement specifically, more specifically, the present invention relates to a kind of method removing cholesterol in animal tallow.
Background technology
Cholesterol in animal grease exists with free and combined two kinds of forms, and the cholesterol of combined is the cholesteryl ester of hydroxyl by free fatty acids esterification, such as cholesterol acid ester or cholesterol cetylate etc. The general cholesterol containing 0.25%-0.3% in butterfat, 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.
It is well known that very high serum cholesterol content, hypertension, abnormal electrocardiogram figure etc. are the important factors causing heart trouble to show effect. Much research in recent years finds that high-content plasma cholesterol can cause atherosclerosis, and coronary heart disease danger is strengthened. In human body, high-content serum cholesterol major cause has the familial hypercholesterolemia of heredity conjunction chaotic, assorted and often eats high saturated fatty-calorie-cholesterol diet. Nutrition and fitness guru think that the cholesterol level in keeping on a diet also is an important step while of being the first step of prevention and therapy hypercholesterolemia and hypolipidemic. Therefore, in research reduction food, cholesterol level especially reduces cholesterol level in animal tallow and causes the interest of many investigators.
CN101292020 discloses a kind of method adopting sterol in adsorbent grease, and wherein said sorbent material comprises clay, silicon-dioxide or their mixture. Sterol wherein is the material that a class comprises cholesterol (free cholesterol and cholesteryl ester) and plant sterol.
US5128162 (A) adopts and will contain sweet three ester oils and many units acylting agent generation esterification of cholesterol; obtain the mixture of sweet three ester oils of cholesterol base monoesters, unreacted many unit's acyl reagent and cholesterol level reduction that polarity becomes big; then unreacted many units acyl reagent it is separated; remaining mixture and parting material are reacted; reclaim sweet three ester oils, obtain eliminating sweet three ester oils of cholesterol. In this method, many units acylting agent is as the reactant of esterification, comprises cyclic acid anhydride and polyprotonic acid halogenide etc., the catalyzer that free acid reacts as this. The shortcoming of this method: (1) reactant system is complicated, it is necessary to additionally add reactant. (2) complex operation step; because esterification after product polarity becomes big; needing to add the mode such as alkaline aqueous solution or anionite-exchange resin to remove, unnecessary many units acylting agent also needs washing or centrifugal or solvent extraction to remove in addition, industrialization can operational degree low.
Therefore, it is necessary to provide a kind of de-method except total cholesterol in grease newly, 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 de-method except total cholesterol in grease newly, the especially de-method except total cholesterol in animal tallow, the removing cholesterol rate adopting the method relatively prior art removing cholesterol rate increase significantly.
The object of the invention is to provide a kind of de-method except cholesterol in animal tallow.
The de-method removing cholesterol in animal tallow provided by the invention comprises the following steps:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs, obtains esterification products;
(2) adsorb: by esterification reaction product and adsorbent contact, obtain adsorbed product;
(3) it is separated: adsorbed product is carried out solid-liquid separation.
In a preference, described in be separated into centrifugation, natural subsidence separation, separatory separation or filtering separation.
In another preference, esterification comprises chemical method esterification, enzyme method esterification.
In another preference, chemical method esterification reaction temperature is 130 ~ 250 DEG C, and enzyme method esterification temperature is 20 ~ 110 DEG C.
In another preference, animal tallow is contacted by chemical method esterification process with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 130 ~ 250 DEG C, or after contact forms mixture, regulates temperature to 130 ~ 250 DEG C of described mixture.
In another preference, chemistry 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, chemistry catalyst for esterification reaction consumption is the 0.01% ~ 2% of animal tallow weight, it is preferable that 0.3% ~ 1%.
In another preference, chemistry reaction time of esterification is 0.5 ~ 12h.
In another preference, animal tallow is contacted by enzyme method esterification process with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 20 ~ 110 DEG C, or after contact forms mixture, regulates temperature to 20 ~ 110 DEG C of described mixture.
In another preference, enzyme method catalyst for esterification reaction is one or more in lipase, esterification enzyme.
In another preference, enzyme method catalyst for esterification reaction consumption is the 0.1% ~ 20% of animal tallow weight.
In another preference, enzyme method reaction time of esterification is 0.5 ~ 24h.
In another preference, absorption reaction temperature is 100-200 DEG C.
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, adsorbent amount is the 0.5% ~ 10% of animal tallow weight, it is preferable that 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 wherein contained free cholesterol.
In another preference, described animal tallow be selected from fish oil, lard, butter, chicken fat, duck fat, butterfat one or more, it is preferable that animal tallow be selected from fish oil, lard, butter or its combination.
In some the preferred embodiments adopting aforementioned method, the step that esterification reaction product is carried out first time separation is also comprised before being also included in absorption reaction, preferably, first time separation can be centrifugation, natural subsidence separation, separatory separation or filtering separation.
Nutritionist advise be grown up every day cholesterol intake should lower than 300mg, to cardiovascular patient, should lower than 200mg. Especially 2008, Ministry of Health's notice was printed and distributed in " Food Nutrition Labeling management regulation " and the content requirement of cholesterol is limited. So, the de-cholesterol level removed or reduce in hypercholesterolemia food is needed for market.
Therefore, it is also an object of the present invention to provide a kind of animal tallow.
Animal tallow provided by the invention is according to the above-mentioned de-animal tallow prepared except the method for total cholesterol in animal tallow.
It is also an object of the present invention to provide the purposes of this animal tallow.
The animal fat of the present invention is for the preparation of food or medicine.
The method of the present invention has the following advantages:
(1) the inventive method is without the need to adding extra reaction substrate, without the need to removing unnecessary reactant in later separation treatment step, simple to operate;
(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 only adopting absorption method.
Embodiment
" scope " disclosed herein is with the form of lower limit and the upper limit. One or more lower limit can be respectively, and one or more upper limit. Given range is limited 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 carry out by this way limiting comprise and may be combined with, and namely any lower limit can be combined to form a scope with any upper limit. Such as, the scope of 60-120 and 80-110 is listed for special parameter, it is to understand that for the scope of 60-110 and 80-120 is also expected in advance. In addition, if the minimum extent value listed 1 and 2, and if list maximum range value 3,4 and 5, then the scope below can all be expected in advance: 1-3,1-4,1-5,2-3,2-4 and 2-5.
In the present invention, unless otherwise indicated, new technical scheme can be mutually combined to form between the content range of each component of composition and its preferable range.
In the present invention, unless otherwise indicated, " its combination " represents the multicomponent mixture of described each element, such as two kinds, three kinds, four kinds and until the multicomponent mixture of maximum possible.
In the present invention, unless otherwise indicated, all " part " and percentage ratio (%) all refers to weight percentage.
In the present invention, unless otherwise indicated, in all compositions, the percentage ratio sum of each component is 100%.
In the present invention, unless otherwise indicated, numerical range " a-b " represents that the contraction table of any real combinings between a to b is shown, wherein a and b is real number. Such as numerical range " 0-5 " represents the whole real numbers all listing between " 0-5 " herein, and the contraction table that " 0-5 " is these combinations of values is shown.
If do not particularly not pointed out, this specification sheets term " one " used refers to " at least one ".
If do not particularly not pointed out, the benchmark that percentage ratio of the present invention (comprises weight percentage) is all the gross weight of described composition.
Herein, unless otherwise explanation, the ratio of each component or weight all refer to dry weight.
In the present invention, if do not illustrated especially, all enforcement modes mentioned in this article and preferred implementation can be combined to form new technical scheme mutually.
In the present invention, if do not illustrated especially, all technology features mentioned in this article and preferred feature can be combined to form new technical scheme mutually.
In the present invention, if do not illustrated especially, mentioned in this article can sequentially carry out in steps, it is also possible to carry out at random, but preferably order carries out. Such as, described method comprises step (a) and (b), represents that described method can comprise step (a) and (b) that order carries out, it is also possible to comprise step (b) and (a) that order carries out. Such as, described mention described method and also can comprise step (c), represent that step (c) random order can join described method, such as, described method can comprise step (a) and (b) and (c), also step (a), (c) and (b) can be comprised, it is also possible to comprise step (c), (a) and (b) etc.
In the present invention, if do not illustrated especially, " comprising " mentioned in this article represents open, it is also possible to be closed. Such as, described " comprising " other elements that can also comprise and not list can be represented, it is also possible to only comprise the element listed.
In the present invention, if do not illustrated especially, concrete numerical value in embodiment hereof and concrete material can with other integrate features describing part herein. Such as, the temperature that description part herein mentions reaction is 10-100 DEG C, and the temperature of reaction that embodiment is mentioned is 20 DEG C, so can think the scope having specifically disclosed 10-20 DEG C herein, or the scope of 20-100 DEG C, and this scope can describe part other integrate features get up to form new technical scheme. Again such as, description part herein mentions a compounds alcohol, and the concrete alcohol that embodiment is mentioned is ethanol, and so ethanol can get up form new technical scheme with other integrate features of description part.
Method
The present invention provides a kind of de-method except cholesterol in grease, and described method comprises the following steps:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs, obtains esterification reaction product;
(2) adsorb: by esterification reaction product and adsorbent contact, obtain adsorbed product;
(3) it is separated: adsorbed product is carried out solid-liquid separation.
In the present invention, term " separation " refers to method or the process of the two-phase (such as solid phase and liquid phase) being divided into separation by the mixture (such as esterification reaction product and/or or adsorbed product) obtained. to those skilled in the art, for reaching the object of separation, the separation method that can adopt is conventional, the those of ordinary skill of this area also directly can be determined in conjunction with prior art according to description of the invention again, such as, the difference of the aspects such as the density including but not limited to utilize material or utilize the difference of the granular size of material or utilize the difference etc. of the permeability of material to be separated, specifically, the separation method that can adopt in the present invention includes but not limited to centrifugation, natural subsidence is separated, separatory separation or filtering separation, in these methods, the concrete parameter vision method used is different and distinguishes to some extent, but to those skilled in the art, it is all conventional, the those of ordinary skill of this area also directly can be determined in conjunction with prior art according to description of the invention again.
In the present invention, if do not illustrated especially, " animal tallow " as herein described or " animal fat " refer to be derive from animal and contain fat or the grease of cholesterol, specifically, include but not limited to, fish oil, lard, butter, chicken and duck fat, butterfat or its combination.
In the present invention, if do not illustrated especially, " cholesterol " as herein described is the derivative of a kind of perhydrocyclopentanophenanthrene, it is present in lipoprotein in blood, and it is several that its existence form comprises high density lipoprotein cholesterol, low density lipoprotein cholesterol, extra-low density protein cholesterol. Also having cholesterol in animal tallow, be there is impact by its content in the quality of animal grease.
In the present invention, if do not illustrated especially, " free cholesterol " as herein described refers to the cholesterol that free state form exists, the cholesterol particularly existed with free state form in animal grease.
In the present invention, if do not illustrated especially, " combined cholesterol " as herein described refers to the cholesteryl ester being combined with lipid acid, the cholesteryl ester being particularly combined in animal grease with lipid acid.
In the present invention, if do not illustrated especially, " total cholesterol " as herein described refers to free state cholesterol and the general designation of combined cholesterol.
In the present invention, esterification refers to that alcohol follows carboxylic acid or oxygen-containing inorganic acid to generate the reaction of ester and water, esterification needs to add catalyzer usually with accelerated reaction, and according to the difference of the catalyzer used, esterification can comprise chemical method esterification, enzyme method esterification etc.
In the present invention, if not having special explanation, chemical method esterification as herein described refers to that alcohol follows carboxylic acid or oxygen-containing inorganic acid to generate the reaction of ester and water under the effect of chemical catalyst. In the present invention, " chemical catalyst " refers to and presents its natural form or be rendered as and the catalyst substance of the carrier prepared according to technology well known by persons skilled in the art or the form of mixtures of matrix. " chemical catalyst " that use in the esterification reaction is well known to those skilled in the art, it is possible to the chemical catalyst for esterification includes but not limited to an acidic catalyst, basic catalyst etc. Specifically, include but not limited in aluminum oxide, aluminium hydroxide, silicon-dioxide, Vanadium Pentoxide in FLAKES, phosphoric acid etc. one or more. Preferably, it may also be useful to aluminum oxide including, but not limited to ��-Al2O3����-Al2O3����-Al2O3Deng or its their mixture or composition. The technician of this area can also according to the teachings of the present invention, it may also be useful to other chemical catalysts reported in existing document.
In the present invention, if there is no special explanation, enzyme method esterification as herein described refers to that alcohol follows carboxylic acid or oxygen-containing inorganic acid to generate the reaction of ester and water under the katalysis of specific biological enzyme, can be used for the enzyme of katalaze enzyme method esterification is conventional for a person skilled in the art, comprise the various enzyme that can be used for catalytic esterification, such as can one or more in lipase, esterification enzyme, specifically, it is possible to include but not limited to Lipozyme435, LipozymeRMIM, LipozymeTLIM.
In another preference, chemical method esterification reaction temperature is 130 ~ 250 DEG C, and enzyme method esterification temperature is 20 ~ 110 DEG C.
In another preference, animal tallow is contacted by chemical method esterification process with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 130 ~ 250 DEG C, or after contact forms mixture, regulates temperature to 130 ~ 250 DEG C of described mixture.
In another preference, animal tallow is contacted by enzyme method esterification process with esterifying catalyst.
In another preference, before contact, described animal tallow temperature is adjusted to 20 ~ 110 DEG C, or after contact forms mixture, regulates temperature to 20 ~ 110 DEG C 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 method catalyst for esterification reaction consumption is the 0.1% ~ 20% of animal tallow weight.
In another preference, enzyme method reaction time of esterification is 0.5 ~ 24h.
In the present invention, " absorption " refer to that material (mainly solid matter) surface holds the phenomenon of a certain component in surrounding medium (liquid or gas) or some component. To those skilled in the art, liquid (such as grease) adds sorbent material (normally having the solid matter of adsorption), so that the specific components (particularly impurity) in this liquid is removed maybe by the target components enrichment in this liquid, it is a kind of routine techniques means. In the present invention, " sorbent material " be any can by with molecules of interest direct interaction or be attached on sorbent material compound interact and by another kind of species adsorbs to the solid-state and fixing material on its surface. To those skilled in the art, for reaching the object of absorption, the method that can adopt is conventional, and the those of ordinary skill of this area also directly can be determined in conjunction with prior art according to description of the invention again. Such as, it may also be useful to sorbent material be well known in the art and can easily be obtained by commercial sources, can be such as one or more in carclazyte, gac, silicon-dioxide, Trisyl. When using sorbent material to adsorb, the amount etc. of the sorbent material of the adsorption temp adopted, adsorption time that absorption reaction carries out, use to those skilled in the art, is conventional, or on the basis of content disclosed by the invention, directly determine in conjunction with prior art.
In the present invention, the silicon-dioxide that can use is including, but not limited to silica, precipitated silica, fumed silica, silica gel, soft silica and mixture thereof etc.; " carclazyte " refers to that with clay (mainly wilkinite) be raw material, and through mineral acid treatment, then through the sorbent material that water rinse, drying are made, but the carclazyte that can use in the present invention includes but not limited to use aforesaid method to obtain; " Trisyl " as herein described is a kind of silica gel hydrogel. But the 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 DEG C, preferably 110-200 DEG C, 120-200 DEG C, 130-200 DEG C, 140-200 DEG C, 150-200 DEG C, 160-200 DEG C, 170-200 DEG C, 180-200 DEG C, 190-200 DEG C, 100-190 DEG C, 110-190 DEG C, 120-190 DEG C, 130-190 DEG C, 140-190 DEG C, 150-190 DEG C, 160-190 DEG C, 170-190 DEG C, 180-190 DEG C, 100-180 DEG C, 110-180 DEG C, 120-180 DEG C, 130-180 DEG C, 140-180 DEG C, 150-180 DEG C, 160-180 DEG C, 170-180 DEG C, 100-170 DEG C, 110-170 DEG C, 120-170 DEG C, 130-170 DEG C, 140-170 DEG C, 150-170 DEG C, 160-170 DEG C, 100-160 DEG C, 110-160 DEG C, 120-160 DEG C, 130-160 DEG C, 140-160 DEG C, 150-160 DEG C, 100-150 DEG C, 110-150 DEG C, 120-150 DEG C, 130-150 DEG C, 140-150 DEG C, 100-140 DEG C, 110-140 DEG C, 120-140 DEG C, 130-140 DEG C, 100-130 DEG C, 110-130 DEG C, 120-130 DEG C, 100-120 DEG C, 110-120 DEG C, 100-110 DEG C.
In a preference of the present invention, the time of described absorption reaction is 1 ~ 120min, it is 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, adsorbent amount is the 0.5% ~ 10% of animal tallow weight (W/W), it is preferable that 1% ~ 10%, 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 wherein contained free cholesterol.
In another preference, described animal tallow wide material sources, it can be such as the grease in one or more sources included but not limited in fish, bird and/or beasts, preferably, include but not limited to be selected from fish oil, lard, butter, chicken fat, duck fat, butterfat one or more, it is more preferable to ground 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 the oil of separation from fish, including, but not limited to grass carp oil, carp oil, crucian oil, seal oil, shark oil shai, cittle fish oil, octopus oil, flatfish oil, sardine oil, perch oil, whale oil, salmon oil, cod oil, mullet oil, oceanic bonito oil etc., comprise their mixture and composition.
In some preferred embodiments adopting aforementioned method, before absorption reaction, also comprise the step that esterification reaction product is separated (i.e. first time separation, being separated into " separation " or " second time separation " after corresponding absorption reaction).
To those skilled in the art, for reaching the object of separation, the separation method that can adopt in " first time separation " step can be conventional, the those of ordinary skill of this area also directly can be determined in conjunction with prior art according to description of the invention again, such as, the difference of the aspects such as the density including but not limited to utilize material or utilize the difference of the granular size of material or utilize the difference etc. of the permeability of material to be separated, specifically, the separation method that can adopt in " first time separation " step of the present invention includes but not limited to centrifugation, natural subsidence is separated, separatory separation or filtering separation, in these methods, the concrete parameter vision method used is different and distinguishes to some extent, but to those skilled in the art, it is all conventional, the those of ordinary skill of this area also directly can be determined in conjunction with prior art according to description of the invention again.
Product and purposes
Present invention also offers the animal fat of animal tallow and the preparation using the method for the present invention to prepare for the preparation of the purposes of food or medicine.
Useful effect
The method of the present invention has the following advantages:
(1) the inventive method is without the need to adding extra reaction substrate, without the need to removing unnecessary reactant in later separation treatment step, simple to operate;
(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 only adopting 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, the those of ordinary skill of this area can directly determine the concrete constant stirred again according to description of the invention in conjunction with prior art, so that free fatty acids and free cholesterol in animal tallow fully react under the effect of catalyzer. 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, the various raw materials of the present invention all can be obtained by commercially available; Or the ordinary method according to this area prepares. Unless otherwise defined or described herein, the same meaning that all specialties used herein and science term and those skilled in the art are familiar with. 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, the present invention is described in detail, but the scope of the present invention is not limited thereto.
Raw material
Trisyl: purchased from Grace company;
SiO2: purchased from Chemical Reagent Co., Ltd., Sinopharm Group;
Active A l2O3: purchased from my fourth reagent (Shanghai) company limited;
Atlapulgite: purchased from Mt. Huang in Anhui Tai Ke activated Fuller earth company limited;
The enzyme used: purchased from Novozymes Company;
Fish oil: purchased from TASA company of Peru;
Lard, butter, butterfat are all purchased from special oil (Shanghai) company limited in good;
Chicken and duck fat is purchased from Nong Pi market, the Five continents, Shanghai City.
Detection method
Total cholesterol detects: GB/T9695.24-2008 meat quail 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 DEG C, adds sorbent material, react 1 ~ 120min under vacuum. Reaction is centrifugal after terminating makes its solid-liquid separation, gets liquid phase, obtains being stripped of the animal grease of part free cholesterol and total cholesterol.
The experiment condition that comparative example 1 is respectively tested and experimental result are in table 1.
Table 1: the experiment condition of comparative example 1 and experimental result
Comparative example 2:
Animal grease is heated, adds 1% (weight) SiO2Make catalyzer, vacuum tightness 5mbar, carry out esterification 1h at 180 DEG C. Centrifugal make its solid-liquid separation, get liquid phase. Then other cholesterol reduction methods reporting (extracting the technique research. Hu Wenna of cholesterol from lanosterol, Zhejiang University's master thesis [D], 2011.) are adopted to remove total cholesterol. Concrete grammar is as follows: get the oil phase after above-mentioned separation, adds the dehydrated alcohol that volume ratio is 1:1 under normal temperature, and extraction 10min, leaves standstill separatory, and getting upper oil phase continuation interpolation volume ratio is the dehydrated alcohol of 1:1, repeats aforesaid operations 3 times. Get oil phase rotary evaporation, remove the dehydrated alcohol of residual, the total cholesterol level in oil phase after detection rotary evaporation.
The de-method except cholesterol of extraction after above-mentioned first esterification, only adopts the extraction of dehydrated alcohol method in contrast. Getting animal grease, add the dehydrated alcohol that volume ratio is 1:1 under normal temperature, extraction 10min, leaves standstill separatory, and getting upper oil phase continuation interpolation volume ratio is the dehydrated alcohol of 1:1, repeats aforesaid operations 3 times. Get oil phase rotary evaporation, remove the dehydrated alcohol of residual, the total cholesterol level of the oil phase after detection 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, after the first esterification of employing, the total cholesterol decreasing ratio of the method for extraction treatment is identical with the total cholesterol decreasing ratio of direct extraction treatment. Namely other cholesterol reduction methods beyond absorption method are not effective pre-treatment conditions by esterification, can not increase the effect of follow-up cholesterol reduction.
Embodiment 1:
Chemical method esterification+absorption
Being heated by animal grease, add catalyst for esterification reaction, at a certain temperature, vacuum tightness keeps below 10mbar to carry out esterification for some time. After this reaction system has been reacted, centrifugal make solid-liquid separation, get liquid phase; Then above-mentioned animal grease is heated to 100��200 DEG C, adds sorbent material, react 1��120 minute under vacuum condition. The reaction of this reaction system is taken out filter and is made solid-liquid separation, obtain low total cholesterol and the animal grease of low free cholesterol after terminating. The experiment condition of embodiment 1 is in table 3.
Table 3: the experiment condition of embodiment 1
In embodiment 1, each experimental result compares in table 4 with comparative example 1 result.
Table 4: each experimental result of embodiment 1 compares with comparative example 1 experimental result
By table 4 result it may be seen that 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 most high energy improves more than 10 times.
Embodiment 2
Esterification+the absorption of enzyme method
Being heated by animal grease, add enzyme method catalyst for esterification reaction, at a certain temperature, vacuum tightness keeps below 10mbar to carry out esterification for some time. After this reaction system has been reacted, centrifugal make solid-liquid separation, get liquid phase; Then the liquid phase obtained in previous step is heated to 100��200 DEG C, adds sorbent material, react 1��120 minute under vacuum condition. The reaction of this reaction system is taken out filter and is made solid-liquid separation, obtain low total cholesterol and the animal grease of low free cholesterol after terminating. The experiment condition of embodiment 2 is in table 5.
The experiment condition of table 5 embodiment 2
In embodiment 2, each experimental result compares in table 6 with comparative example 1 result.
Table 6: each experimental result of embodiment 2 compares with comparative example 1 experimental result
By table 6 result it may be seen that adopt enzyme method 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 aforementioned method, for avoiding the impact on absorption, it is separated after esterification. For investigating the impact of this step, corresponding grease is processed again by contriver respectively by the method for embodiment 1 and 2, but directly use esterification products to carry out adsorption operations after esterification, instead of use the liquid product carrying out solid-liquid separation acquisition in advance to adsorb, detect the decreasing ratio of free cholesterol and total cholesterol respectively, and the free cholesterol of grease processed with the grease processed by the method for embodiment 1 and 2 and carrying out with existing method and the decreasing ratio of total cholesterol compare.
Experimental result shows, and 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 of the correlation method adopting embodiment 1 and 2. But grease is processed by the method adopting embodiment 3, the decreasing ratio of its total cholesterol and free cholesterol is still obviously higher than the decreasing ratio of total cholesterol and free cholesterol when adopting a step absorption method, even finding, in best result, removing cholesterol rate improves 8 times.
The foregoing is only the better embodiment of the present invention, and it is not used to limit the substantial technological context of the present invention, the substantial technological content of the present invention is broadly defined in the right of application, any technology entities that other people complete or method, if with application right define completely identical, or the change of a kind of equivalence, also all it is covered by being regarded as among this right.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document. In addition it will be understood that after the foregoing having read the present invention, the present invention can be made various changes or modifications by those skilled in the art, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (18)
1. a de-method except total cholesterol in animal tallow, described method comprises the following steps:
(1) esterification: animal tallow, under the effect of catalyzer, esterification occurs; Described esterification is add the SiO of the heavy 1%-2% of animal tallow2Make catalyzer and chemistry esterification occurs, or add the lipase as catalyst generation enzyme method esterification that animal tallow weighs 1% 20%;
(2) adsorb: esterification reaction product and adsorbent contact, obtain adsorbed product;
(3) it is separated: adsorbed product is carried out solid-liquid separation;
Described esterif iotacation step is not additionally added reaction substrate.
2. the method for claim 1, it is characterised in that, also comprise a step: before absorption reaction, esterification reaction product is carried out first time separation, to obtain liquid phase after esterification.
3. method as claimed in claim 1 or 2, it is characterised in that, described in be separated into centrifugation, natural subsidence separation, separatory separation or filtering separation.
4. the method for claim 1, it is characterised in that, described contact is for join described sorbent material in described esterification reaction product.
5. the method for claim 1, it is characterised in that, before described contact, regulate esterification reaction product temperature, or after esterification reaction product and adsorbent contact form mixture, regulate the temperature of described mixture.
6. the method for claim 1, it is characterised in that, the esterification of described chemistry for be adjusted to 130��250 DEG C by described animal tallow temperature before contact, or regulates described mixture temperature to 130��250 DEG C after the two contact forms mixture; Described enzyme method esterification for be adjusted to 20��110 DEG C by described animal tallow temperature before contact, or regulates temperature to 20��110 DEG C of described mixture after the two contact forms mixture.
7. the method for claim 1, it is characterised in that, described chemistry reaction time of esterification is 0.5��12h.
8. the method for claim 1, it is characterised in that, the reaction times of described enzyme method esterification is 0.5��24h.
9. the method for claim 1, it is characterised in that, the adsorption temp of step (2) is 100��200 DEG C.
10. the method for claim 1, it is characterised in that, the adsorption time of step (2) is 1��120min.
11. the method for claim 1, it is characterised in that, described sorbent material is one or more in carclazyte, gac, silicon-dioxide, Trisyl.
12. the method for claim 1, it is characterised in that, the consumption of described sorbent material is the 0.5%��10% of animal tallow weight.
13. methods as claimed in claim 12, it is characterised in that, the consumption of described sorbent material is the 2%��10% of animal grease weight.
14. the method for claim 1, it is characterised in that, in described animal tallow, the mol ratio of contained free fatty acids and the free cholesterol contained by it is more than or equal to 0.5:1.
15. methods as claimed in claim 14, it is characterised in that, described animal tallow is selected from fish oil, lard, butter, chicken and duck fat, butterfat or its combination.
16. methods as claimed in claim 15, it is characterised in that, described animal tallow is selected from fish oil, lard, butter or its combination.
Animal tallow prepared by 17. methods as according to any one of claim 1-16.
18. animal tallows as claimed in claim 17 are for the preparation of the purposes of food or medicine.
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| NO20181574A1 (en) * | 2018-12-06 | 2020-06-08 | Epax Norway As | Very long chain fatty acids |
| 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 |
| 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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