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WO2010003457A1 - Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses - Google Patents

Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses Download PDF

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Publication number
WO2010003457A1
WO2010003457A1 PCT/EP2008/058942 EP2008058942W WO2010003457A1 WO 2010003457 A1 WO2010003457 A1 WO 2010003457A1 EP 2008058942 W EP2008058942 W EP 2008058942W WO 2010003457 A1 WO2010003457 A1 WO 2010003457A1
Authority
WO
WIPO (PCT)
Prior art keywords
fat
container
sample
soxhlet
sample container
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.)
Ceased
Application number
PCT/EP2008/058942
Other languages
English (en)
Inventor
Henrik Thomsen
Christian Born
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.)
Foss Analytical AS
Original Assignee
Foss Analytical AS
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 Foss Analytical AS filed Critical Foss Analytical AS
Priority to PCT/EP2008/058942 priority Critical patent/WO2010003457A1/fr
Publication of WO2010003457A1 publication Critical patent/WO2010003457A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0288—Applications, solvents
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction

Definitions

  • the present invention relates to a sample container and a method of determining the fat content of a sample.
  • An established conventional laboratory method for determination of the amount of fat (which herein shall be defined as including all fatty acids and all lipids, such as wax, oil and other lipophilic molecules) in a sample of food, feed or foodstuff (hereinafter a sample) is based on variants of the Soxhlet method.
  • the principal steps of a common variant of the method, allowing determination of the total of bound and unbound fat include placing a well known amount of sample in an appropriate container, subjecting the sample to hydrolysis by boiling acid to release the bound fat, rinsing the sample, drying the sample and finally extracting the fat by a heated solvent such as diethyl ether or petroleum ether and determining the total amount of fat by weighing it. If determination of unbound fat is required separately an additional extraction must be completed prior to hydrolysis, and similarly if only unbound fat is known to be present hydrolysis may be omitted.
  • 6492:1999 6492:1999, and other variants are implemented commercially, such as the method marketed by FOSS Analytical under the commercial name Soxtec.
  • FOSS Analytical for analysis of milk products an alkaline hydrolysis is used due to the special characteristics of milk.
  • the present invention relates to the hydrolysis and extraction steps of the Soxhlet method, and to a sample container appropriate for use in this method.
  • the sample container is an important element in the practical operation of the hydrolysis and the subsequent extraction.
  • the container must be able to retain the liberated fat while the hydrolysis acid is allowed to diffuse through a filter into the container; during drying the fat must also be retained, but during extraction the fat of the sample dissolved in solvent must be allowed to pass through the filter, while the non-extractable solids of the sample is retained.
  • the glass frit sample container and the hydrolysed sample is dried in an oven or a microwave oven. After the hydrolysed sample has been dried, extraction of the fat with solvent must take place. The free fat will be dissolved in solvent, and due to the low viscosity the mixture will flow freely through the glass frit. To ensure complete and rapid extraction with a minimum consumption of solvent, the solvent is heated and refluxed. After extraction solvent is separated from the fat by evaporation or, in the case of reusing the solvent, distillation, and the remaining fat is weighed to obtain the total amount of fat in the sample. After completion the glass frit must be thoroughly cleaned to avoid that residues from previous samples are blocking the glass frit pores. While the use of a glass frit container is beneficial from the point of view of labour requirements during analysis, the glass frit container is costly and is most often reused, which requires time consuming cleaning.
  • WO 02/33403 A disclose that the Soxhlet method may be carried out using a sample container comprising a filter plug from a porous filtration material, wound in a spiral placed inside a glass or plastic tube and a paper filter thimble - here called a thimble and filter plug container.
  • a sample container comprising a filter plug from a porous filtration material, wound in a spiral placed inside a glass or plastic tube and a paper filter thimble - here called a thimble and filter plug container.
  • the disclosed method instructs that the container is turned over and that the filter plug is rearranged and a secondary filter - a paper thimble - is used for filtration to separate sample from fat solubilised in solvent.
  • the thimble and filter plug container has the benefit of a low cost, and is therefore suited for single use, but it has the drawbacks that the volume of water retained in the filtration material is high due to the thickness of the filter plug, which requires extra time for drying, and furthermore, that several manual steps are required, both in the production of the container and in the operation of the method.
  • the present invention is intended overcome some or all of the problems listed above, and specifically to reduce the amount of manual handling involved in determination of fats in biological materials.
  • a first aspect of the invention is a means of filtration for use in a Soxhlet sample container
  • a second aspect is a Soxhlet sample container
  • a third aspect is a method for determination of fat in a sample.
  • the filter materials appropriate for use in the invention must fulfil multiple criteria.
  • a first criterion is that the materials must be able to withstand the conditions during the Soxhlet process, including hot acid or base during hydrolysis and hot solvent during extraction.
  • the filter must be permeable to polar liquids such as acid, base and water, and during extraction the filter must be permeable to solvent and solubilised fats.
  • the filter must show sufficient fat retaining capacity to retain substantially all the fat present in the sample analysed.
  • non-woven polymeric materials such as but not limited to polyethylene (PE), polypropylene (PP), polyester (PET), polyamide (PA), and polyamide-6 (PA6), which possibly may be produced or treated by special methods to enhance certain characteristics of the filter materials, such as increasing the hydrophilicity and the permeability to polar liquids.
  • Suitable treatment methods include chemical treatments such as addition of surfactants, as well as physical methods such as ion bombardments, plasma treatments and ozone treatments.
  • the filter materials may also be a woven polymer, a metallic mesh and woven or non woven glass fibres, possibly treated by suitable means to obtain the required characteristics.
  • a test container is made by attaching a disc of filter material 220 in a container with a mechanical fastening means 230 as shown in Fig.2.
  • the internal diameter of the container body 210, and accordingly the diameter of the active filter area was 32 mm.
  • test container is filled with 5 ml of rape seed oil, and is held above a surface to allow the filter to drip until no drops are observed for 60 seconds.
  • Fig.1 shows a Soxhlet sample container with a permanently attached filter
  • Fig.2 shows a Soxhlet sample container with a filter fixed by a screw thread union
  • Fig.3 shows a Soxhlet sample container with two layers of filter material
  • Fig.4 shows a Soxhlet sample container with three layers of filter material.
  • a Soxhlet sample container appropriate for single use is made from a filter 120 made from a disc of filter material permanently attached to a cylindrical container body 110, by melting the two parts together by a heating source, such as a contact heating element, infrared heating, ultrasonic heating, lasers or friction.
  • a heating source such as a contact heating element, infrared heating, ultrasonic heating, lasers or friction.
  • the filter material 120 is preferably a non-woven mixture of polyethylene and polypropylene, which in the same configuration, supports hydrolysis by allowing an unaided flow of acid, base and water while retaining fat and supports extraction of fat by allowing an unaided flow of solvent and solubilised fat in solvent.
  • a porous filter with an ability to absorb and thus retain fat may often also retain water and may therefore require a longer time for rinsing away acid and drying and therefore it is beneficial if the porous filter is having a thickness of less than 5 mm, preferably less than 2 mm, and more preferably less than 1 mm.
  • a sheet of filter material 220 is attached to a container body 210 by a mechanical fastening means 230, such as a union fastened by a screw thread, a bayonet coupling or spring loaded coupling which seals the sheet of filter material 220 against the container body 230.
  • a mechanical fastening means 230 has the advantage of supporting a re-use of the container body 210, while allowing the filter material 220 to be discarded.
  • An appropriate Soxhlet sample container may also be produced by insert moulding or by production from a pouch of filter material, where the container walls are made impermeable by an appropriate treatment such as covering the walls with an appropriate material or sintering by heat.
  • the means of filtration comprises multiple layers of filter materials with different functionality but the dominant fat retaining ability is due to a single material, which is preferably in a thin layer, for the reason discussed above, and which for simplicity is called the fat retaining filter layer.
  • Fig.3 is shown a third embodiment of the invention, having the benefit that the risk of the sample blocking the flow is reduced, by removing the sample 350 from immediate contact with the fat absorbing filter 320.
  • the Soxhlet sample container according to this embodiment of the invention comprises a container body 310 and two layers of filter material 320, 330.
  • a thin fat retaining filter material layer 320 is attached to the bottom of the container body 310, and a thicker coarse filter 330 is placed above this, separating the sample 350 from the fat retaining filter material 320.
  • Fig.4 a fourth embodiment of the invention is shown, wherein the means of filtration comprises 3 layers of filter materials, with potential production and handling benefits.
  • a coarse grid 440 at the bottom of the container body 410 has the main function of supporting a thin plug of fat retaining filter material layer 420.
  • the optional coarse filter 430 has the same function of separating the fat absorbing filter material 420 from the sample 450.
  • This embodiment has the benefit during production that the container body 410 and the coarse grid 440 may be moulded from one material, and that a thin plug of the fat retaining filter material 420 may be placed without requiring production equipment, for instance in the case where it is desired that the body of the Soxhlet sample container is reused.
  • a method of testing a fat content of an item comprising one or more of the following steps
  • steps (i) to (e) are included for full compatibility with the ISO method and to allow the separate determination of unbound and bound fat, and may be excluded, especially for a known sample type.
  • steps (b) to (e) are included for full compatibility with the ISO method and to allow the separate determination of unbound and bound fat, and may be excluded, especially for a known sample type.
  • steps (b) to (e) are included for full compatibility with the ISO method and to allow the separate determination of unbound and bound fat, and may be excluded, especially for a known sample type.
  • the use of cold water may be beneficial to avoid mixing of fats and water, and thus leakage of fats through the means of filtration.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

L'invention concerne un procédé de détermination des matières grasses dans un échantillon, un récipient pour échantillon pour extracteur de type Soxhlet et un moyen de filtration (120, 220, 320, 420) utilisable dans un récipient pour échantillon pour extracteur de type Soxhlet. Ledit moyen de filtration est caractérisé en ce qu'il est conçu pour favoriser l'hydrolyse en permettant le passage sans assistance d'un flux d'acide, de base et d'eau tout en retenant les matières grasses, ainsi que pour favoriser l'extraction des matières grasses en permettant le passage sans assistance d'un flux de solvant et de matières grasses solubilisées dans ledit solvant.
PCT/EP2008/058942 2008-07-09 2008-07-09 Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses Ceased WO2010003457A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/EP2008/058942 WO2010003457A1 (fr) 2008-07-09 2008-07-09 Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2008/058942 WO2010003457A1 (fr) 2008-07-09 2008-07-09 Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses

Publications (1)

Publication Number Publication Date
WO2010003457A1 true WO2010003457A1 (fr) 2010-01-14

Family

ID=40456244

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2008/058942 Ceased WO2010003457A1 (fr) 2008-07-09 2008-07-09 Récipient pour échantillon utilisable dans le cadre de la détermination des matières grasses

Country Status (1)

Country Link
WO (1) WO2010003457A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5858178A (en) * 1994-03-22 1999-01-12 Lautenschlaeger; Werner Process and device for preparing and/or extracting samples using a vaporizable agent at high temperature
WO1999002959A1 (fr) * 1997-07-07 1999-01-21 University Of Bristol Contenant poreux
WO2002033403A2 (fr) * 2000-10-16 2002-04-25 Foss Tecator Ab Recipient de filtration
US6479295B1 (en) * 1999-05-04 2002-11-12 Andrew R. Komarek Method for determining fat (crude) in feed, food, and other materials utilizing filter media encapsulation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5858178A (en) * 1994-03-22 1999-01-12 Lautenschlaeger; Werner Process and device for preparing and/or extracting samples using a vaporizable agent at high temperature
WO1999002959A1 (fr) * 1997-07-07 1999-01-21 University Of Bristol Contenant poreux
US6479295B1 (en) * 1999-05-04 2002-11-12 Andrew R. Komarek Method for determining fat (crude) in feed, food, and other materials utilizing filter media encapsulation
WO2002033403A2 (fr) * 2000-10-16 2002-04-25 Foss Tecator Ab Recipient de filtration

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