Fractionation process

Organic compounds -- part of the class 532-570 series – Organic compounds – Fatty compounds having an acid moiety which contains the...

Reexamination Certificate

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C554S008000, C554S206000, C554S211000, C426S417000

Reexamination Certificate

active

06552208

ABSTRACT:

The present invention refers to a new process for fractionation of vegetable oils giving a confectionary fat as well as a product enriched in unsaponifiable components.
BACKGROUND OF THE INVENTION
In the fractionation of vegetable oils to obtain a main fraction suitable for the manufacture of confectionary fats different liquid side fractions are also obtained. Said side fractions, the composition of which varies with the starting oil and the fractionation conditions, have been used in the food industry, for example for the preparation of emulsifiers, but are in general regarded as of little value.
It is well known that vegetable oils and fats contain a large number of biologically active components in addition to the dominating triglycerides. Such components are for instance polar lipids, that is phospholipids, sphingolipids and galactolipids, as well as more or less nonpolar lipid components such as phytosterols, triterpene alcohols and aliphatic alcohols, tocopherols, vitamin E for instance, and tocotrienols. The unsaponifiable part of the oil, by definition the material from a lipid sample which can be extracted by petroleum ether or diethyl ether after alkaline hydrolysis, is typically said to comprise said nonpolar to semi-polar lipids, hydrocarbons and waxes.
The unsaponifiable components of many vegetable oils are known to have different properties of interest for use in cosmetic and pharmaceutical preparations (Wachter, R., et al., Phytosterole—pflanzliche Wirkstoffe in der Kosmetik, Parfümerie und Kosmetik, 75. Jahrgang, Nr. 11/94). The natural content and composition of the unsaponifiable lipid components in vegetable oils is unique for each raw material. The functionality of different concentrates enriched in unsaponifiable product is explained by the respective composition of said components, mainly tocopherols, phytosterols and triterpene esters.
Shea butter, for instance, has an unusually high content of unsaponifiable matter, up to 13%, hydrocarbons inclusive. The unsaponifiable lipids of shea butter are characterized by a high content of UV-absorbing triterpene esters and natural phytosterols claimed to impose anti-inflammatory effects on damaged skin.
The unsaponifiable lipids of rapeseed oil are dominated by a unique high content of sterols, such as &bgr;-sitosterol, campesterol and brassicasterol, as well as tocopherols known to offer a good natural protection against oxidation. An unsaponifiable fraction of rapeseed oil has proven to show an anti-inflammatory effect on irritated skin (Lodén, M., et al., Effect of topically applied lipids on surfactant-irritated skin, British Journal of Dermatology 1996; 134: 215-220).
In the manufacturing of raw material for the food industry many of the unsaponifiable components in the vegetable fat or oil are negatively affected by the processing conditions and others are removed. The content of unsaponifiable components varies with the origin of the raw material. Typically the non glyceride part of a refined oil amounts to 0.5-1.0% by weight.
In order to obtain the unsaponifiable, biologically active components of interest there are different ways to proceed. The oil can for instance be saponified and components of interest extracted, which process will however produce large amounts of fatty acids and glycerol. In addition some of the components, for instance esters of sterols and triterpene alcohols will become saponified and lose their oil solubility. Another method is steam distillation of the oil and processing of the distillate. In this method the oil is under low pressure blown with steam which takes away volatile components, more or less, depending on the pressure and the temperature. However, also triglycerides and fatty acids are taken away and the. distillate has to be subjected to a saponification and extraction procedure, alternatively to a short path distillation, in order to purify the components of interest. By this the activity and quality of the components are reduced. Still another method is to fractionate the oil in a suitable solvent at a low temperature. This is a preferred process as the active components can be obtained or concentrated without being chemically modified.
PRIOR ART
Processes for fractionating oils and fats have since long been used for the manufacturing of confectionary fats or hard butters and also for obtaining fractions having certain specific characteristics. The liquid products which are obtained as by-products have been used in the food industry. In the processing of a vegetable oil one or more of the following steps are normally used:
pressing or extraction of the raw material;
refining of the pressed or extracted oil, that is degumming with acid to remove the polar lipids, deacidification with alkali to remove free fatty acids, and bleaching to reduce colour and oxidation products;
catalytic hydrogenation;
solvent fractionation of the hydrogenated oil bringing the triglycerides to precipitate;
deodorization by means of steam to remove components that give rise to unwanted flavours and odours.
U.S. Pat. No. 2,972,541, for instance, refers to hard butters and a method for preparing said hard butters by solvent fractionation from oils composed of essentially triglycerides of fatty acids of 16 and 18 carbon atoms. In order to recover triglycerides of interest the starting oil is hydrogenated to convert the fatty acid radicals of the oil from cis to trans figuration and to lower the initial unsaturation by eliminating most of the polyethenoic unsaturation. The hydrogenated oil can then be solvent fractionated, a technique well known in the glyceride oil art, to give a crystalline hard butter fraction. Nothing is, however, stated about the unsaponifiable fraction or the content of non-triglycerides in the oil.
EP-B1-0690904 refers to a process for the preparation of fractions of a fat of vegetable origin enriched with unsaponifiable materials, which process is characterized in that the fat is treated with a polar solvent such as acetone and heated giving a first fraction insoluble in hot solvent which is rich in unsaponifiable material. Said first fraction can be combined with a second fraction obtained from the soluble fraction after crystallization thereof at a temperature below 0° C., preferably at −15 to −30° C., filtration and evaporation of the filtrate. The obtained fraction enriched in unsaponifiable material is said to be useful for the preparation of cosmetical and pharmaceutical compositions, but nothing is stated about the utility of the solid fractions. The fat described is shea butter.
WO 96/03137 refers to cosmetic and pharmaceutical preparations containing shea butter concentrates having an increased content of components which can not be saponified. Said shea concentrates have been produced from raw or refined shea butter by distillation in a short path distiller at a temperature of 200-300° C. and at a reduced pressure. It is also said to be possible to produce adequate concentrates by extraction of shea butter with organic solvents such as ethanol. In this process the original composition of the unsaponifiable components will, however, be destroyed as the esters are hydrolysed, oxidised and/or isomerised.
There is still a need of a process from which it will be possible to obtain, in addition to one or more hard fractions suitable for confectionary applications, a useful side fraction, such as a liquid fraction rich in chemically unaltered, unsaponifiable, biologically active components from vegetable oils in a cost effective way.
DESCRIPTION OF THE INVENTION
The present invention refers to a process for fractionation of a vegetable oil in order to obtain one or more steeply melting solid fractions suitable for confectionary applications as well as a liquid fraction rich in unsaponifiable, biologically active components.
In order to prepare confectionary fats, as well as a fraction rich in unsaponifiable, biologically active components, from a vegetable oil the oily raw material should be treated by the following steps in any suitable order: —pretre

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