EP2429306A1 - Process for the preparation of marine oils - Google Patents

Process for the preparation of marine oils

Info

Publication number
EP2429306A1
EP2429306A1 EP10713469A EP10713469A EP2429306A1 EP 2429306 A1 EP2429306 A1 EP 2429306A1 EP 10713469 A EP10713469 A EP 10713469A EP 10713469 A EP10713469 A EP 10713469A EP 2429306 A1 EP2429306 A1 EP 2429306A1
Authority
EP
European Patent Office
Prior art keywords
marine
marine oil
oil
temperature
oils
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP10713469A
Other languages
German (de)
French (fr)
Other versions
EP2429306B1 (en
Inventor
Otto Eduard Rosier
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Upfield Spreads UK Ltd
Unilever NV
Flora Food Global Principal BV
Original Assignee
Unilever PLC
Unilever NV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unilever PLC, Unilever NV filed Critical Unilever PLC
Priority to EP10713469.4A priority Critical patent/EP2429306B1/en
Publication of EP2429306A1 publication Critical patent/EP2429306A1/en
Application granted granted Critical
Publication of EP2429306B1 publication Critical patent/EP2429306B1/en
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/16—Refining fats or fatty oils by mechanical means
    • 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
    • C11B3/00—Refining fats or fatty oils
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter

Definitions

  • the present invention relates to a process for the preparation of marine oils, in particular marine oils such as fish oil, algae and/or microbial oils and concentrates thereof .
  • marine oils in particular marine oils and/or microbial oils and marine oils/concentrates, may be free of odor and smell when fresh, but reversion through oxidation occurs very rapidly.
  • Another object of the invention is to improve the keepability of marine oil. Another object of the present invention is to bring marine oil in a form wherein it remains pumpable after storage without the unacceptable formation of sediment and without the need for winterization.
  • the present invention involves a process for the handling and storage of marine oils comprising the steps of: (a) optionally heating the marine oil to a temperature of
  • the oil prepared according to the invention is a non- winterized marine oil i.e. an oil which is easily oxidized, developing off-taste.
  • marine oils are: fish oils for example obtained from fatty fish such as mackerel, salmon, tuna, squid, whale, menhaden, pilchard, anchovy, sardine and herring, or microbial oils as algae oil, obtained from marine micro algae or krill oil.
  • the marine oil has an iodine value of 100 or more, more preferably 120 or more.
  • the marine oil has a C20+C22 content of lwt.% or more. More preferably the marine oil is fish oil, such as oil from Tuna, Herring, salmon, tuna, Menhaden, anchovy, sardines, Skipjack or concentrates made thereof.
  • Marine oils as used in the present invention may be refined according to well-known refining procedures like neutralization to remove the free fatty acids, bleaching to remove colored components and contaminants, and deodorization to remove odiferous components. Variations on the existing procedures are also well known. Fatty acids can also be physically removed by means of a short path distillation equipment.
  • the bleaching step can also be carried out in various manners. Silica, carbon and bleaching earth in various grades and concentrations are frequently used in the bleaching step.
  • the marine oils of the invention preferably are non- winterized marine oils generally having a solid fat content (SFC) of 5 to 25 wt% % at 5 C, preferably 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%.
  • SFC is a well known parameter of fat and can be determined by conventional methods. It will be appreciated that the SFC at 5 C of the marine oil may vary depending on the source and the natural variation of the marine oil, but generally a SFC at 5 C of 5 wt% or more for marine oils is indicative of the non-winterized nature of said marine oil.
  • the first step of the process of the invention involves the optional heating of the marine oil to a temperature of 20-45 C to ensure that the marine oil is fully liquid.
  • the heating step (a) can be omitted and the liquid oil can directly be used in the other steps of the process.
  • the fully liquid marine oil is cooled in a scraped surface heat exchanger to a temperature of -5 tolO C.
  • Scraped surface heat exchangers are commonly used in the processing and cooling of food products such as oils, icecream and margarine and are often referred to as so-called A units.
  • a units are conveniently used in the second step of the invention whereby the fully liquid marine oil is cooled to a temperature of -5 to 10 C, preferably to a temperature of 0-10 C, more preferably from 1 to 10 C.
  • the time to effect the cooling may vary but will generally be from 5 to 1000 seconds, more general from 10 to 100 seconds.
  • the rate of cooling in the second step is from 0.1 to 1 degree per second, for example 0.5 to 2 C per second. If appropriate two or more A units may be used for example for sequential cooling.
  • step (b) After the cooling of step (b) the cooled marine oil is maintained in a steered vessel at a temperature of 3-lOC for a period of 1-10 minutes.
  • a commonly used steered vessel in the food industry is a pin-steered unit which is often referred to as a C-unit.
  • a C-unit is used in step c for maintaining the cooled marine oil.
  • more than one C-unit can be used for the steered maintenance, for example 2 A units may be used for cooling while 2 C units may be used for steered keeping, for example in the sequence A C A C.
  • the keeping time in the steered vessel is 15 seconds to 10 minutes while the temperature is maintained at a low temperature of 1-10 C, for example 2-6 minutes.
  • the marine oil thus obtained is filled in a container, for example an oil drum, where after the container is closed and stored below 15 C for example in the cooled state (say at 3-10 C) .
  • the suspension thus obtained does not suffer from an unacceptable increase in viscosity and/or sedimentation upon storage at ambient temperature.
  • the present invention relates to a marine oil obtainable by the process as described above.
  • Said marine oil is characterized by a solid fat content at 5 C of from 5 to 25 wt% in combination with a viscosity at
  • SFC at 5 C of said marine oil is from 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%.
  • the oil was cooled in 32 seconds to 5C in an A unit followed by maintenance in a C-unit at 5C for 264 seconds.
  • the resulting suspension was filled into pre-cooled containers at 5C and stored at this temperature. After 28 hours of storage the suspension still was liquid and has a viscosity of 650 mPa.s measured at 10 C and 30 rpm.
  • Example 1 was repeated while using a fish oil having a SFC of 9.7 but omitting step c (maintenance in the C-unit) .
  • the resulting fish oil was fully solid after storage and the viscosity could not adequately be determined at 10 C.
  • the fish oil of example 2 was cooled and stored in accordance to the method of example 1.
  • the resulting suspension was after storage still fully liquid and has a viscosity at 10 C and 30 rpm of 676 mPa.s.
  • EXAMPLE 4 (invention) A fish oil obtained from Ocean Nutrition Canada and having a SFC of 5.7 wt% at 5C was processed in accordance to example 1 resulting after storage in a liquid suspension having a viscosity of 600 mPa.s at 30 rpm and 10 C.
  • EXAMPLE 5 (comparison)
  • Example 2 was repeated while using the fish oil of example 4, resulting in a solid fish oil composition for which the viscosity at 10 C could not adequately be determined.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Edible Oils And Fats (AREA)
  • Fats And Perfumes (AREA)

Abstract

A process for the handling and storage of marine oils comprising the steps of: (a) optionally heating the marine oil to a temperature of 20-45 C to ensure that the marine oil is fully liquid; (b) Cooling the fully liquid marine oil in one or more scraped surface heat exchangers to a temperature of -5-10 C; (c) maintaining the cooled marine oil obtained in step (b) in one or more a steered vessels at a temperature of -5-10 C for a total period of 1-10 minutes; (d) Storing the marine oil thus obtained in a closed container at a temperature below 15 C.

Description

PROCESS FOR THE PREPARATION OF MARINE OILS
Field of the invention
The present invention relates to a process for the preparation of marine oils, in particular marine oils such as fish oil, algae and/or microbial oils and concentrates thereof .
Background to the invention
Recently the use of marine oils as food ingredients has attracted increased interest especially because of the presence of long chain fatty acids such as EPA and DHA.
It is well known that these marine oils, in particular marine oils and/or microbial oils and marine oils/concentrates, may be free of odor and smell when fresh, but reversion through oxidation occurs very rapidly.
Many attempts have been made to stabilize marine oils. For example a common method is to store and transport the marine oils at low temperature, for example in the frozen state. At these low temperatures the marine oils are solid and are less prone to degradation effects. However the storage in the frozen form has the disadvantage that long periods are needed for the freezing and the thawing of the product leading to an undesired increase in storage time. Also the freezing of the oil and the subsequent transport at low temperature requires an undesired ongoing input of energy. Another problem in the storage and transport of marine oils is the fact that marine oils tend to solidify during storage and/or transport at ambient temperature. Such solidification renders the marine oil less suitable for handling under factory conditions because the solid oil can generally not be pumped at ambient temperature or the oil requires an undesired heating step before it can be handled.
Another problem in the storage and transport of marine oils is the fact that marine oils due to their relative high solid fat content tend to form a solid fat and wax containing phase which during storage and transport often sediments to the bottom of the storage vessel. This sediment generally is non-pumpable and therefore cannot be used under standard factory conditions. In practice therefore this sediment layer is often discarded as waste leading to an undesired loss of material and an increase of costs .
Winterization has been used to separate the solid fat from the marine oil prior to storage or transport. This indeed may result in a decrease of the above problems of solidification and sedimentation, however winterization causes an undesired delay and also leads to the removal of the hard fat fraction, which -unless a suitable economic use of this solid fat fraction can be found- significantly increases the cost of the resulting winterized marine oil. Summary of the invention
It is therefore an object of the invention to improve the keepability of marine oil. Another object of the present invention is to bring marine oil in a form wherein it remains pumpable after storage without the unacceptable formation of sediment and without the need for winterization.
Surprisingly it has been found that a specific cooling regime for the marine oil leads to the formation of a stable suspension of a solid fat fraction in a liquid fraction without the occurrence of undesired solidification and sedimentation and without the need of prior winterization.
Accordingly the present invention involves a process for the handling and storage of marine oils comprising the steps of: (a) optionally heating the marine oil to a temperature of
20-45 C to ensure that the marine oil is fully liquid;
(b) Cooling the fully liquid marine oil in one or more scraped surface heat exchangers to a temperature of -5-10 C;
(c) maintaining the cooled marine oil obtained in step
(b) in one or more a steered vessels at a temperature of -5-10 C for a total period of 15 seconds to 10 minutes; (d) Storing the marine oil thus obtained in a closed container at a temperature below 15 C. Detailed description of the invention
The oil prepared according to the invention is a non- winterized marine oil i.e. an oil which is easily oxidized, developing off-taste. Examples of marine oils are: fish oils for example obtained from fatty fish such as mackerel, salmon, tuna, squid, whale, menhaden, pilchard, anchovy, sardine and herring, or microbial oils as algae oil, obtained from marine micro algae or krill oil. Preferably the marine oil has an iodine value of 100 or more, more preferably 120 or more. Preferably the marine oil has a C20+C22 content of lwt.% or more. More preferably the marine oil is fish oil, such as oil from Tuna, Herring, salmon, tuna, Menhaden, anchovy, sardines, Skipjack or concentrates made thereof.
Marine oils as used in the present invention may be refined according to well-known refining procedures like neutralization to remove the free fatty acids, bleaching to remove colored components and contaminants, and deodorization to remove odiferous components. Variations on the existing procedures are also well known. Fatty acids can also be physically removed by means of a short path distillation equipment. The bleaching step can also be carried out in various manners. Silica, carbon and bleaching earth in various grades and concentrations are frequently used in the bleaching step.
The marine oils of the invention preferably are non- winterized marine oils generally having a solid fat content (SFC) of 5 to 25 wt% % at 5 C, preferably 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%. SFC is a well known parameter of fat and can be determined by conventional methods. It will be appreciated that the SFC at 5 C of the marine oil may vary depending on the source and the natural variation of the marine oil, but generally a SFC at 5 C of 5 wt% or more for marine oils is indicative of the non-winterized nature of said marine oil.
The first step of the process of the invention involves the optional heating of the marine oil to a temperature of 20-45 C to ensure that the marine oil is fully liquid.
It will be appreciated that if the starting oil is already fully liquid at ambient temperature, for example because a fully fresh oil is used, the heating step (a) can be omitted and the liquid oil can directly be used in the other steps of the process.
In the second step of the process of the invention the fully liquid marine oil is cooled in a scraped surface heat exchanger to a temperature of -5 tolO C.
Scraped surface heat exchangers are commonly used in the processing and cooling of food products such as oils, icecream and margarine and are often referred to as so-called A units. A units are conveniently used in the second step of the invention whereby the fully liquid marine oil is cooled to a temperature of -5 to 10 C, preferably to a temperature of 0-10 C, more preferably from 1 to 10 C. Depending on the size of the scraped surface exchanger the time to effect the cooling may vary but will generally be from 5 to 1000 seconds, more general from 10 to 100 seconds. Preferably the rate of cooling in the second step is from 0.1 to 1 degree per second, for example 0.5 to 2 C per second. If appropriate two or more A units may be used for example for sequential cooling.
After the cooling of step (b) the cooled marine oil is maintained in a steered vessel at a temperature of 3-lOC for a period of 1-10 minutes.
A commonly used steered vessel in the food industry is a pin-steered unit which is often referred to as a C-unit. Preferably a C-unit is used in step c for maintaining the cooled marine oil. If desired more than one C-unit can be used for the steered maintenance, for example 2 A units may be used for cooling while 2 C units may be used for steered keeping, for example in the sequence A C A C.
The keeping time in the steered vessel is 15 seconds to 10 minutes while the temperature is maintained at a low temperature of 1-10 C, for example 2-6 minutes.
After the cooling for example in an A-unit and maintaining the oil, for example in a C-unit, the marine oil thus obtained is filled in a container, for example an oil drum, where after the container is closed and stored below 15 C for example in the cooled state (say at 3-10 C) .
Surprisingly it has been found that the above process leads -even after 28 hours of storage to products which have a low viscosity. Generally products obtained by the process of the invention are uniquely characterized by a combination of a relatively high SFC (solid fat content) and a relatively low viscosity of less than 1000 mPa.s at 30 rpm at 10 C. Although applicants do not wish to be bound by any theory it is believed that the specific processing sequence of the invention leads to the formation of an under cooled marine oil after step b wherein little to no fat crystals are yet formed, while step C results in the controlled crystallization of said under cooled marine oil leading to the formation of a stable suspension of small fat crystals with little to no crystal growth upon storage in the remainder of the liquid marine oil.
Surprisingly the suspension thus obtained does not suffer from an unacceptable increase in viscosity and/or sedimentation upon storage at ambient temperature.
In a second aspect the present invention relates to a marine oil obtainable by the process as described above.
Said marine oil is characterized by a solid fat content at 5 C of from 5 to 25 wt% in combination with a viscosity at
30 rpm and 10 C of less than 1000 mPa.s. Preferably the
SFC at 5 C of said marine oil is from 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%.
The invention will now be illustrated by means of the following examples.
Viscosity measurement A Brookfield Rotovisco meter Model DV-I+ was used to measure viscosity. Spindle LV3 was chosen as measuring probe. The viscosity was measured by lifting the sample and make sure the spindle was covered by the oil precisely to the indication level on the spindle, applying 30 rpm and waiting for 1 minute to read the viscosity at that shear rate.
EXAMPLE 1 (invention)
Fish oil obtained from Ocean Nutrition and having an SFC of 10.2 at 5C was heated to 40 C and processed as follows:
the oil was cooled in 32 seconds to 5C in an A unit followed by maintenance in a C-unit at 5C for 264 seconds. The resulting suspension was filled into pre-cooled containers at 5C and stored at this temperature. After 28 hours of storage the suspension still was liquid and has a viscosity of 650 mPa.s measured at 10 C and 30 rpm.
EXAMPLE 2 (comparison)
Example 1 was repeated while using a fish oil having a SFC of 9.7 but omitting step c (maintenance in the C-unit) . The resulting fish oil was fully solid after storage and the viscosity could not adequately be determined at 10 C.
EXAMPLE 3 (invention)
The fish oil of example 2 was cooled and stored in accordance to the method of example 1. The resulting suspension was after storage still fully liquid and has a viscosity at 10 C and 30 rpm of 676 mPa.s.
EXAMPLE 4 (invention) A fish oil obtained from Ocean Nutrition Canada and having a SFC of 5.7 wt% at 5C was processed in accordance to example 1 resulting after storage in a liquid suspension having a viscosity of 600 mPa.s at 30 rpm and 10 C. EXAMPLE 5 (comparison)
Example 2 was repeated while using the fish oil of example 4, resulting in a solid fish oil composition for which the viscosity at 10 C could not adequately be determined.

Claims

Claims
1. A process for the handling and storage of marine oils comprising the steps of: (a) optionally heating the marine oil to a temperature of 20-45 C to ensure that the marine oil is fully liquid;
(b) Cooling the fully liquid marine oil in one or more scraped surface heat exchangers to a temperature of -5-10 C;
(c) maintaining the cooled marine oil obtained in step (b) in one or more a steered vessels at a temperature of -5-10 C for a total period of 15 seconds to 10 minutes; (d) Storing the marine oil thus obtained in a closed container at a temperature below 15 C.
2. Process according to claim 1, wherein step (b) is carried out in one or more A units and step (c) in one or more C-units
3. Process according to claim 2, involving the use of 2 or more A units for cooling and 2 or more C units for steering.
4. Process according to claim 1, wherein the marine oil is a fish oil having an SFC at 5 C of 5 to 25 wt%, preferably 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%.
5. Marine oil suspension obtainable by the process of claim 1, 2 or 3.
6. Marine oil obtainable by a process according to claim 1 having a SFC at 5 C of from 5 to 25 wt% and having after storage for 24 hours at 10 C a viscosity at 1OC and 30rpm of less than 1000 mPa.s.
7. Marine oil according to claim 6 having a SFC at 5 C of from 5 to 20 wt%, more preferably 5 to 17 wt% and even more preferably 5 to 12 wt%.
EP10713469.4A 2009-05-13 2010-04-14 Process for the preparation of marine oils Not-in-force EP2429306B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP10713469.4A EP2429306B1 (en) 2009-05-13 2010-04-14 Process for the preparation of marine oils

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP09160088 2009-05-13
PCT/EP2010/054887 WO2010130517A1 (en) 2009-05-13 2010-04-14 Process for the preparation of marine oils
EP10713469.4A EP2429306B1 (en) 2009-05-13 2010-04-14 Process for the preparation of marine oils

Publications (2)

Publication Number Publication Date
EP2429306A1 true EP2429306A1 (en) 2012-03-21
EP2429306B1 EP2429306B1 (en) 2017-01-04

Family

ID=41037707

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10713469.4A Not-in-force EP2429306B1 (en) 2009-05-13 2010-04-14 Process for the preparation of marine oils

Country Status (5)

Country Link
EP (1) EP2429306B1 (en)
CA (1) CA2761632C (en)
CL (1) CL2011002836A1 (en)
PE (1) PE20121039A1 (en)
WO (1) WO2010130517A1 (en)

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2999022A (en) * 1957-03-26 1961-09-05 Anderson Clayton & Co Liquid shortening method
GB1025992A (en) * 1962-07-16 1966-04-14 Unilever Ltd Fat compositions and their preparation
US5211981A (en) * 1991-06-13 1993-05-18 The Procter & Gamble Company Process for making a uniform liquid, pourable shortening containing high emulsifier levels
US5436021A (en) * 1992-12-31 1995-07-25 Van Den Bergh Co., Division Of Conopco, Inc. Pumpable oleaginous compositions
US6033703A (en) * 1993-06-24 2000-03-07 The Procter & Gamble Company Beta-stable low-saturate, low trans, all purpose shortening
NZ500703A (en) * 1998-11-04 2001-06-29 F Preparation of food-grade marine edible oils by treatment with silica, vacuum steam deodorisation and addition of a herb extract

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2010130517A1 *

Also Published As

Publication number Publication date
WO2010130517A1 (en) 2010-11-18
EP2429306B1 (en) 2017-01-04
PE20121039A1 (en) 2012-08-04
CA2761632C (en) 2018-02-27
CA2761632A1 (en) 2010-11-18
CL2011002836A1 (en) 2012-07-20

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