WO2018109203A2 - Fractionnement bidimensionnel de matière grasse de lait - Google Patents

Fractionnement bidimensionnel de matière grasse de lait Download PDF

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Publication number
WO2018109203A2
WO2018109203A2 PCT/EP2017/083137 EP2017083137W WO2018109203A2 WO 2018109203 A2 WO2018109203 A2 WO 2018109203A2 EP 2017083137 W EP2017083137 W EP 2017083137W WO 2018109203 A2 WO2018109203 A2 WO 2018109203A2
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Prior art keywords
fat
fractionation
fraction
fractionate
milk
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PCT/EP2017/083137
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English (en)
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WO2018109203A3 (fr
Inventor
Franciscus Johannes Gerardus Boerboom
William Kloek
Cynthia Akkermans
Reza RANJBAR DAVIJANI
Michiel Scheffer
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Frieslandcampina Nederland B.V.
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Application filed by Frieslandcampina Nederland B.V. filed Critical Frieslandcampina Nederland B.V.
Priority to CN201780077429.2A priority Critical patent/CN110072984A/zh
Priority to EP17825810.9A priority patent/EP3555254A2/fr
Publication of WO2018109203A2 publication Critical patent/WO2018109203A2/fr
Publication of WO2018109203A3 publication Critical patent/WO2018109203A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0008—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents
    • C11B7/005—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of solubilities, e.g. by extraction, by separation from a solution by means of anti-solvents in solvents used at superatmospheric pressures
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
    • C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points

Definitions

  • the invention relates to a process for preparing a fat fractionate from a fat composition comprising milk fat. Further, the invention relates to a fat fraction. Further, the invention relates to a method for preparing a food product, comprising the use a fat fractionate according to the invention.
  • Milk fat is complex mixture of triglycerides and other lipid components. Milk fat typically consists for the largest part of triglycerides (e.g. about 98 %).
  • the triglycerides generally have a carbon number in the range of 26-54. In particular for milk fat from cow milk, usually, the carbon number distribution is bimodal, i.e.
  • milk fat has fatty acids with a relatively high content of relatively small acyl groups (4-6 carbons), a relatively high content of relatively large acyl groups (at least 14 carbons) and a relatively low content of acyl groups of intermediate length (8- 12 carbons),
  • milk fat typically contains several minor components, such as cholesterol, fat-soluble vitamins, free fatty acids, monoglycerides, diglycerides and various other organic components, such as lactones, ketones and aldehydes, contributing to the characteristic flavour or aroma of milk fat.
  • milk fat contains various highly nutritious components. However, not all ingredients of milk fat are appreciated for their nutritional value. Furthermore, milk fat has characteristic physical properties, e.g. melting range and structural functionalities, e.g. consistency, spreadability and the like. Such properties are desirable for specific applications, but not necessarily so for others. For example, milk fat may be used as a substitute for cocoa-butter in chocolate products or chocolate imitation products (compounds). However, increasing incorporation of milk fat in such products may cause undesirable softening, changes in tempering conditions, gloss or contraction.
  • a common process is milk fat fractionation on the basis of melt temperature (dry fractionation, also known as melt crystallisation). This process can be a single-step fractionation or a multi-step fractionation. In each
  • fractionation step a liquid phase (marked as '0' for Olein', because this fraction typically is enriched in oleic acid (bound as triglyceride), indicative of long-chain unsaturated fatty acid content) and a solid phase (marked as 'S' for 'stearin' because this fraction typically is enriched in stearic acid (bound as triglyceride), indicative of long-chain fatty acid content).
  • a liquid phase marked as '0' for Olein', because this fraction typically is enriched in oleic acid (bound as triglyceride), indicative of long-chain unsaturated fatty acid content
  • solid phase marked as 'S' for 'stearin' because this fraction typically is enriched in stearic acid (bound as triglyceride), indicative of long-chain fatty acid content.
  • SO is the fluid fraction obtained after the dry fractionating the solid fraction from a first dry fractionation step
  • SS would be the solid fraction after that second fractionation step.
  • OOO is the fluid fraction of a triple dry fractionation process wherein the liquid phase of a first fractionation (O) was subjected to a second dry fractionation step and the liquid phase of the second fractionation (00) was subjected to a third fractionation. OOS would then be the solid fraction of that third fractionation.
  • Dry fractionation is for instance used to produce butter having superior spreading properties and the production of milk fat fractions for use in bakery applications. It has also been proposed to use a solid fraction of a dry fractionation process in the production of chocolate products, for instance to replace cocoa butter or to change the texture of chocolate but so far literature shows that this has not yet been successful.
  • Supercritical fluid fractionation also known as supercritical fluid extraction of liquids
  • has been proposed as an alternative to dry fractionation see also the above identified review by Hamm and paper by Arul et al. With this process a raffinate and a distillate is obtained.
  • Supercritical fluid fractionation is thought to fractionate fats primarily on the basis of molecular weight.
  • EP 74145 Al is an example of a patent application relating to a process wherein supercritical fluid fractionation is used to produce a mixture of triglycerides having butter-like properties.
  • the ratio is an example of a patent application relating to a process wherein supercritical fluid fractionation is used to produce a mixture of triglycerides having butter-like properties.
  • saturated/unsaturated acyl groups in the fractions can also be altered in a different way than this ratio is altered in dry fractionation.
  • fat compositions at least majorly based on milk fat, having specific properties, such as a nutritional value, specific structural properties, specific flavour/aroma properties and the like, as desired for a particular application.
  • alternative fat compositions based at least majorly on milk fat.
  • fat compositions that more closely resemble mother milk than conventional milk fat fractions. Such compositions are particularly interesting for formulating infant formulas and toddler food products.
  • alternative flavouring/aroma compositions based on milk fat.
  • alternative fat compositions that are regarded as having a highly nutritional value (e.g. high content of mono- or polyunsaturated fatty acids), yet have another property that is generally thought to be associated with fat components considered less healthy, such as high melting point.
  • the invention relates to a process for preparing a fat fractionate, comprising
  • the invention relates to a process for preparing a fat fractionate, comprising
  • a starting material selected from the group consisting of milk fats and fat mixtures of milk fat and at least one other fat, which fat mixtures are composed of more than 50 wt. % milk fat, preferably at least 90 wt. % milk fat - said starting material preferably being anhydrous -by a supercritical fluid fractionation;
  • the invention further relates to a fat fraction obtainable as a fat fractionate by a process according to the invention.
  • the invention further relates to a method for making a food product, comprising combining a fat fractionate prepared by a process according to the invention or a fat fraction according to the invention with one or more further (usual) food ingredients for making said food product.
  • a process according to the invention is suitable to obtain fat fractions that are different from the starting material and from the intermediate fat fraction in one or more of the following aspects:
  • SAFA saturated fatty acids
  • MUFA monounsaturated fatty acids
  • PUFA polyunsaturated fatty acids
  • n3-polyunsaturated fatty acids concentration of n3- polyunsaturated fatty acids
  • concentration of n3- polyunsaturated fatty acids concentration of one or more fat-soluble vitamins, such as a fat-soluble vitamin selected from the group of vitamin A, vitamin E, vitamin Kl and vitamin K2; concentration of cholesterol; concentration of one or more specific or total lactones; concentration of one or more specific or total ketones; concentration of one or more specific or total aldehydes; concentration of total short-chain fatty acids (C4-C6, abbreviated as SCFA); concentration of total medium-chain fatty acids (C8-C12, abbreviated as MCFA); concentration of total long-chain fatty acids (C14 or higher, abbreviated as LCFA); concentration of total cis-fatty acids; concentration of
  • the fat fractions are different in two or more, more preferably three or more, four or more, five or more, six or more of said aspects.
  • the fat fractions are different in twelve or less, in particular ten or less, more in particular eight or less of said aspects.
  • milk fat as (the major part of) the starting material, compared to a e.g. a plant fat like palm oil, may be a cause of a synergy achievable in accordance with the invention.
  • This complex nature is e.g. reflected in the generally bimodal carbon number distribution of milk fat.
  • the synergistic difference is defined as an enrichment or depletion in one or more of said aspects compared to the starting material, wherein
  • CDF+SC/ Cstart > Cstart+SC / Cstart ⁇ 1 and synergistically depleted is defined as
  • CDF+SC is one of said concentrations in or the carbon number of the fat fractionate obtained by dry fractionation plus the supercritical fluid fractionation of the starting material
  • Cstart is one of said concentrations in or the carbon number of the starting material, such as AMF.
  • Cstart+sc is one of said concentrations in or the carbon number of a fat fraction obtained by only super critical fluid fractionation of the starting material
  • the fat fractionate is enriched in a component or carbon number, usually CDF+SC / Cstart ⁇ 10, in particular CDF+SC / Cstart ⁇ 5, more in particular CDF+SC / Cstan ⁇ 3.5, more in particular CDF+SC /Cstart is about 2.5 or less.
  • the fat fractionate is synergistically depleted CDF+SC / Cstart ⁇ Cstan+sc / Cstan ⁇ 0.9, more preferably CDF+SC / Cstart ⁇
  • Cstart+sc / Cstart ⁇ 0.8 in particular CDF+SC / Cst rt ⁇ Cstan+sc /Cstan ⁇ 0.65. in an Cstan+sc / Cstan ⁇ 0.9.
  • the fat fractionate is depleted in a component or carbon number, usually Cstan+sc / Cstan >0.01, in particular Cstan+sc / Cstan >0.1, more in particular Cstan+sc / Cstan >0.2, more in particular
  • Cstart+SC /Cstart IS about 0.3 ⁇ ⁇ .
  • substantially(ly) or “essential(ly)” is generally used herein to indicate that it has the general character or function of that which is specified. When referring to a quantifiable feature, these terms are in particular used to indicate that it is for at least 75 %, more in particular at least 90 %, even more in particular at least 95 % of the maximum that feature.
  • a product is usually considered essentially free of a substance, in particular water, if the content of the substance is 0- 0.5 wt.%, in particular 0 - 0.2 wt.%, more in particular 0 - 0.1 wt.%, based on total weight of the product in which it is present.
  • certain substances such as certain aromas or
  • the presence in the starting material may be well below 0.5 wt. %, 0.2 wt.% or 0.1 wt. % and still have a significant effect on a property of the product.
  • the term "about” in relation to a value generally includes a range around that value as will be understood by the skilled person. In particular, the range is from at least 15 % below to at least 15 % above the value, more in particular from 10 % below to 10 % above the value, more specifically from 5 % below to 5 % above the value. As used herein, percentages are usually weight percentages unless specified otherwise. Percentages are usually based on total weight, unless specified otherwise.
  • fatty acids these in particular include the fatty acid residues (acyl groups) of triglycerides.
  • the carbon number is determinably by gas chromatography with flame ionization detection (GC-FID), wherein a sample of a substance to be analysed is dissolved in chloroform and injected in the GC. Identification of the carbon numbers and correction factor for the FID response can be done using BCR-632-A sample 160 from Sigma-Aldrich.
  • GC-FID flame ionization detection
  • the starting material is usually essentially water-free.
  • the starting material is usually milk fat, in particular milk fat that is essentially free of water (anhydrous milk fat, abbreviated as 'AMF').
  • AMF can be made in a manner generally known in the art, e.g. using phase inversion and drying.
  • AMF is also commercially available, e.g. from Friesland Campina (Amersfoort, the
  • the milk fat is bovine milk fat, preferably cow milk fat.
  • Buffalo milk fat is another particularly useful starting material.
  • the milk fat may in particular be milk fat from milk of another hoofed ungulate, such as sheep milk fat, goat milk fat or camel milk fat. Of these, goat milk fat is preferred. It is also possible to use a mixture of milk fats from milk from different species of mammals.
  • a minor amount of one or more other fats, in particular one or more fats from a plant or from aquatic organisms (e.g. fish oil, oil from algae).
  • This can be useful, e.g., to provide a starting material with a high mono- or polyunsaturated fatty acid content, e.g. eicosapentaenoic acid (EPA), docosahexanoic acid (DHA) or arachidonic acid (ARA) content .
  • EPA eicosapentaenoic acid
  • DHA docosahexanoic acid
  • ARA arachidonic acid
  • the total content of fat other than milk fat in the starting material usually is 0- 20 wt. %,in particular 1-10 wt.%, more in particular 1-5 wt. %, more in particular 1-2 wt. % . Particularly good results have been achieved with a starting material that consists of milk fat, such as AMF.
  • a desirable fat fractionate for a specific purpose can be obtained in accordance with the invention by a specific combination of two or more subsequent fractionations, at least one being a dry fractionation and at least one being a supercritical fluid fractionation.
  • the dry fractionation conditions and the supercritical fluid fractionation conditions can be based on common general knowledge, the literature cited in the present disclosure, and the contents of the present disclosure, optionally in combination with a limited amount of routine testing.
  • Milk fat fractions obtained by dry fractionation can also be provided by a supplier, from which these are available, e.g. FrieslandCampina (Amersfoort, the Netherlands).
  • the dry fractionation is usually operated under batch conditions.
  • the dry fractionation conditions can generally be based on known conditions, e.g. on the basis of the references mentioned above or the literature cited therein. E.g. The Lipid Handbook, G.D.Gunstone, CRC Pressm, 3 rd Edition, Chapters 4.4.2.4 and 4.4.3, Figure 4.20 and Table 4.17 are indicative of common general knowledge.
  • Figure 1 of the present disclosure illustrates (using AMF from cow milk as an example) how a multiple fractionation results in different fractions, how these fractions are generally named, and how the melting temperatures of the fractions usually relate to each other. It should be noted that the quantitative values are indicative only and may vary, in particular dependent on the composition of the starting material.
  • solvent/feed ratio outlet temperature, pressure, weight to weight ratio distillate to raffinate play a role.
  • supercritical carbon dioxide is particularly suitable, but other known supercritical fluids can be used as an alternative or mixed with carbon dioxide, e.g. one or more supercritical fluids selected from the group of supercritical dinitrogen oxide, supercritical ammonia, supercritical hydrocarbons, supercritical alcohols, halogenated hydrocarbons.
  • supercritical points for such fluids are known, e.g. from EP 744922 Bl.
  • the supercritical conditions can generally be based on known conditions, e.g. on the basis of the references mentioned above or the literature cited therein.
  • the supercritical fractionation can be carried out using equipment that is known per se. It can be a continuous fractionation or a batch fractionation.
  • the temperature of the supercritical medium during fraction may be chosen within a wide range.
  • the temperature is minimally the temperature corresponding to the critical point of the supercritical medium.
  • the temperature is preferably at least 5°C above the critical point, more preferably at least 10°C above the critical point, most preferably at a temperature of at least 15°C above the critical point.
  • the temperature is preferably maximally 100°C, more preferably maximally 80°C, more in particular maximally 70°C.
  • the temperature is usually chosen such that the fat fraction or starting material subjected to supercritical fractionation is fluid, i.e. above the upper end of the melting range. In particular good results have been achieved with supercritical carbon dioxide at a temperature above the critical point in the range of 45-65 °C.
  • the pressure of the supercritical medium may be chosen within a wide range.
  • the pressure is minimally the pressure corresponding to the critical point of the supercritical medium.
  • the pressure is preferably at least 5 bar above the critical point, more preferably at least 10 bar above the critical point.
  • the pressure is usually up to 500 bar above the critical point, in particular 200 bar above the critical point, preferably up to 150 bar above the critical point, in particular up to 100 bar above the critical point.
  • the pressure usually is in the range of 100-250 bar, preferably in the range of 105-200 bar. In particular, good results have been achieved with supercritical carbon dioxide at a pressure above the critical point in the range of 110-140 bar.
  • the solvent/feed ratio can be chosen at a suitable value within a normal operating range for the equipment is used.
  • the ratio is generally chosen high enough to dissolve all of the feed in the supercritical fluid and can be determined empirically. At higher operating pressure, generally a lower solvent/feed ratio is required to dissolve all of the feed.
  • the ratio distillate to raffinate to be a particularly important parameter, to achieve specific, in particular synergistic effects on enrichment or depletion of one or more components of interest.
  • the weight to weight ratio distillate to raffinate based on the total weight of the fat fraction(ate) in the distillate and in the raffinate, in the supercritical fluid fractionation is in the range of 5:95 to 90:10 , preferably in the range of 10:90 to 70:30, in particular in the range of 15:85 to 50:50.
  • a high unsaturated fatty acid content is generally regarded as providing increased nutritional value and tends to have a lowering effect on melting temperature or range.
  • Lactones, ketones and aldehydes generally contribute to a characteristic flavour/aroma.
  • a fluid fraction provided by dry fractionation is used as an intermediate fat fraction from the starting material (if dry fractionation precedes supercritical fluid fractionation), or the fat fractionate is obtained as a fluid fraction of the dry fractionation (if dry fractionation follows supercritical fluid fractionation).
  • the dry fractionation is a multi-step fractionation comprising two or more fractionation steps, wherein the intermediate fat fraction is a solid or fluid fraction obtained after subjecting a fluid fraction of the starting material obtained in a first dry fractionation step is subjected to at least one further dry fractionation step.
  • the fat fractionate is a solid or fluid fraction obtained after subjecting a fluid fraction of an intermediate fat fraction (obtained by supercritical fluid fractionation) which fluid fraction is obtained in a first dry fractionation step to at least one further dry fractionation step.
  • the invention has been found particularly advantageous with respect to fat fractions obtained as a distillate or raffinate, more in particular as a raffinate of the supercritical fluid fractionation in a process according to the invention.
  • a fat fractionate obtained in accordance with the invention may be used as such or be further processed. E.g. it may be subjected to a further fractionation step (dry fractionation, supercritical fractionation or other) or to an
  • a fraction obtained in a process according to the invention that is not to be used for further application e.g. for used in the making of a food product, may be subjected to a further process to recover useful components from the fraction. E.g. it may be recycled into a process of the invention.
  • the prepared fat fraction is obtained from the 0 fraction (the fluid fraction of the first dry fractionation step) of the dry fractionation, which 0 fraction has been subjected to supercritical fluid fractionation or may have been subjected to a further dry fractionation step to yield the intermediate fraction (e.g. OS, 00, OSO, OSS, OOO, OSOO, OOOO, OSSO) that has been subjected to supercritical fluid fractionation.
  • the intermediate fraction e.g. OS, 00, OSO, OSS, OOO, OSOO, OOOO, OSSO
  • fractionation e.g. SO, SS
  • SO sulfur dioxide
  • SS supercritical fluid fractionation
  • the term 'distillate' is used for the distillate of the supercritical fluid fractionation
  • the term raffinate is used for the raffinate of the supercritical fluid fractionation
  • lower melting fraction means olein fractions having a lower melting temperature than the starting material, in particular AMF (typically including 0, 00, 000, 0000 etc.)
  • middle melting fraction means stearin fractions having a lower melting temperature than the starting material, in particular AMF (typically including OS, OOS, OOOS high melting fractions means a higher melting temperature than the starting material, in particular AMF
  • soft fraction means the olein fraction of a dry fractionation
  • hard fraction means the stearin fraction of a dry fractionation
  • a distillate of a lower melting fraction is in particular useful as milk fat product with high amounts of naturally occurring bioactive components important for growth and development, such as fat soluble vitamins, vitamin precursors, cholesterol, etc..
  • a distillate of a lower melting fraction or intermediate melting fraction is in particular useful as fat product containing high concentrations of short chain fatty acids, such as butyric acid, and/or medium chain fatty acids with immunogenic potential.
  • a fat fractionate with enhanced medium chain fatty acids for energy metabolism can be prepared as a distillate of a hard fraction obtained in the dry fractionation.
  • High melting fractions are particularly useful for supercritical fluid fractionation to obtain a fat fractionate that is depleted in palmitic acid, without comprising the functionality thereof.
  • Supercritical fat fractions obtained from hard intermediate fat fractions are particularly useful in the preparation of chocolate or chocolate fantasy products which are more resistant to blooming caused by large temperature fluctuations.
  • Distillates of soft fractions are for instance useful if starting material contains a relatively high trans-fatty acid and a reduction of trans-fatty acid content is desired.
  • a distillate obtained by supercritical fluid fractionation of a middle melting fraction is usually enriched in flavour components, in particular if a dry fractionation fraction is used that is obtained as the liquid fraction in the final dry fractionation step ⁇ e.g. O, OO , OOO, or OOOO).
  • a relatively low weight to weight ratio of distillate to raffinate is preferred for preparing a fat fractionate enriched in aroma components, such as a ratio of 30:70 or less, in particular about 15:80 to 20:80.
  • Such fractionate is particularly useful to impart a butter- like or cream like flavour or aroma to a product or for use as a flavour carrier.
  • a raffinate in particular a raffinate obtained by supercritical fluid fractionation of an intermediate fat fraction obtained by dry fractionation selected from 0, 00, OOO and OOOO, is suitable to provide a fat fractionate more closely resembling the fatty acid composition of human milk. Accordingly, such fractionate is particularly useful for the preparation of an infant formulation or toddler food.
  • a distillate obtained with a process wherein the supercritical fluid fractionation is operated at a relatively low weight to weight ratio distillate to raffinate, such as of about 50:50 or less, is preferred.
  • a raffinate enriched in long chain saturated fatty acid preferably use is made of an intermediate fat fraction obtained by dry fractionation selected from OS and OOO.
  • a distillate of a solid intermediate fraction obtained by dry fractionation is useful (especially S), in particular if the ratio distillate to raffinate is relatively low, such as about 50:50 or less.
  • a supercritical fluid fractionation For enrichment in vitamin A use may be made of a supercritical fluid fractionation with a relatively high ratio distillate to raffinate, such as a ratio of about 50:50 or more.
  • a relatively high ratio distillate to raffinate such as a ratio of about 50:50 or more.
  • supercritical fluid fractionation of the OOO fraction of dry fractionation has been found particularly suitable (with the raffinate as the fat fractionate that is
  • the invention further relates to the preparation of food products using a fat fractionate (obtainable) in accordance with the invention.
  • the food product can generally be prepared in a manner known per se, using known ingredients other than the fat fractionate in known amounts.
  • the fat fractionate will usually replace partly or fully a conventional fat source. E.g. in case chocolate product or chocolate imitation product is prepared, the fat fractionate will usually replace cacao butter or a part thereof.
  • the food product is a chocolate product or a chocolate-imitation product.
  • the food product is an infant formulation.
  • the food product is a medical food product, in particular a clinical nutrition product (i.e. a food product for use in enhancing, maintaining or restoring health and/or prevent a disease, prescribed by a health care professional like a physician, nurse, or dietician, and destined for and supplied to persons in need thereof).
  • the medical food product may be an infant formulation for infants in need of a special nutrition, e.g. for infants suffering from an allergy or metabolic disease.
  • the obtained product is used to manufacture a flavour product or used directly for inclusion in a flavour product.
  • Example 1 The invention will now be illustrated by the following examples.
  • Example 1 The invention will now be illustrated by the following examples.
  • Example 1 The invention will now be illustrated by the following examples.
  • AMF from cow milk was subjected to dry fractionation in a single step fractionation to obtain an 0 and an S fraction, and to multi-step fractionation to obtain various soft and hard fractions, for further fractionation by supercritical fluid fractionation.
  • the dry fractionation process parameters were based on common general knowledge to obtain the fractions.
  • the supercritical C02 extraction took place on a pilot facility with a 4.5 m high and 10 1 capacity column filled with 2 mm stainless steel Raschig rings. The inner diameter of the column was 54mm. In all tests the raw material was fed from the middle of the column (2.25 m from the bottom). First optimal conditions were determined using AMF and dry fractionation fractions as a feed material using batch extraction experiments. Also conditions were determined to achieve different distillate / raffinate ratios.
  • the OOOO fraction and the AMF were subjected to continuous supercritical fractionation; conditions were based on the findings of Example 1.
  • a distillate and a raffinate were obtained under the same conditions. In this case comparable yields of 15% distillate versus 85% of raffinate were obtained for both the AMF and the OOOO fraction.
  • the distillates were analysed by the same FA analysis. In the following table the results are shown.
  • synergy factor for AMF needs to be >1 and the synergy factor for OOOO needs to be larger than for AMF which is both true. So in this case there is synergistic enrichment of butyric acid in these fractions.
  • AMF and an OOOO fraction were prepared as raw materials and analysed on trans fatty acid content by means of fatty acid analysis, as described in Example 2.
  • the OOOO fraction and the AMF were subjected to continuous supercritical fractionation; conditions were based on the findings of Example 1.
  • a distillate and a raffinate were obtained under comparable conditions. In this case comparable yields of 15% distillate versus 85% of raffinate were obtained for both the AMF and the OOOO fraction.
  • the distillates were analysed by the same FA analysis. In the following table the results are shown:
  • synergy factor for AMF needs to be >1 and the synergy factor for OOO needs to be larger than for AMF which is both true. So in this case there is synergistic enrichment of medium chain fatty acids in these fractions.
  • AMF from cow milk
  • OS from cow milk
  • OOO fatty acid
  • the fractions were subjected to continuous supercritical fractionation; conditions were based on the findings of Example 1.
  • a distillate and a raffinate were obtained under comparable conditions. In this case comparable yields of 50% distillate versus 50% of raffinate were obtained for both the AMF and the OOO fraction.
  • the raffinates were analysed by the same FA analysis as in Example 2. In the following table the results are shown:
  • synergy factor for AMF needs to be >1 and the synergy factor for OOO needs to be larger than for AMF which is both true. So in this case there is synergistic enrichment of medium chain fatty acids in these fractions.
  • flavour molecules can be concentrated synergistically by means of supercritical C02 fractionation.
  • AMF from cow milk
  • an OOOO fraction were prepared as raw materials. Equal amounts of these products were put in aluminium coated glass jars at room temperature. These samples were tested blindly by an experienced group of testers familiar with butter and butter products against a standard which was AMF and asked to grade the product on a 5 point scale, 1 clearly less intense, 2: slightly less intense, 3 equally intense, 4: slightly more intense and 5: clearly more intense.
  • the ranking points were collected per person added per sample and summarised in the following table.

Abstract

L'invention concerne un procédé de préparation d'un fractionnat de matière grasse, comprenant la fourniture d'une fraction de matière grasse intermédiaire d'un produit de départ choisi dans le groupe constitué de matières grasses de lait et de mélanges de matières grasses de matière grasse de lait et d'au moins une autre matière grasse, lesdits mélanges de matières grasses étant composés de plus de 50 % en poids de matière grasse de lait, de préférence au moins 90 % en poids de matière grasse de lait, ledit produit de départ étant de préférence anhydre, par un fractionnement à sec ; et la soumission de ladite fraction de matière grasse intermédiaire à un fractionnement de fluide supercritique, le fractionnat de matière grasse étant obtenu sous la forme d'un raffinat du fractionnement de fluide supercritique ou en tant que distillat du fractionnement de fluide supercritique, éventuellement après élimination du fluide supercritique.
PCT/EP2017/083137 2016-12-15 2017-12-15 Fractionnement bidimensionnel de matière grasse de lait WO2018109203A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201780077429.2A CN110072984A (zh) 2016-12-15 2017-12-15 乳脂的二维分馏
EP17825810.9A EP3555254A2 (fr) 2016-12-15 2017-12-15 Fractionnement bidimensionnel de la matière grasse du lait

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