WO2002021101A1 - Method for determining taste and/or smell in liquid or solid products - Google Patents

Method for determining taste and/or smell in liquid or solid products Download PDF

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Publication number
WO2002021101A1
WO2002021101A1 PCT/SE2001/001881 SE0101881W WO0221101A1 WO 2002021101 A1 WO2002021101 A1 WO 2002021101A1 SE 0101881 W SE0101881 W SE 0101881W WO 0221101 A1 WO0221101 A1 WO 0221101A1
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WIPO (PCT)
Prior art keywords
vial
agent
taste
oil
smell
Prior art date
Application number
PCT/SE2001/001881
Other languages
French (fr)
Inventor
Anders HILLSTRÖM
Håkan Palm
Original Assignee
Alfa Laval Corporate Ab
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 Alfa Laval Corporate Ab filed Critical Alfa Laval Corporate Ab
Priority to AU2001284587A priority Critical patent/AU2001284587A1/en
Publication of WO2002021101A1 publication Critical patent/WO2002021101A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02—Food
    • G01N33/03—Edible oils or edible fats
    • 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
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N2030/0095—Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material

Definitions

  • the present invention relates to a method for determining taste and/or smell in liquid or solid vegetable or animal oils and fats, which when heated give off volatile substances.
  • Products where one desires to determine taste and/or smell may consist of different food products in liquid or solid form. For such a determination one uses today often sensory panels, that is persons which have trained their ability to distinguish a certain taste or smell. The experience of a taste or a smell may however be. influenced by different outer circumstances as the form of the day, smoking habits or earlier eaten food. It is also difficult to make an objective comparison between taste or smell experiences made by different test panels.
  • DE 197 58 399 shows how one may use measuring to discover if olive oil or sunflower oil have been- mixed 5 with soybean oil, which is done by analyzing different atomic bonds in the oil sample.
  • DE 43 289 66 describes a method for determining changes in an oil or fat during the time it is used for deep-frying by measuring the ohmic resistance.
  • the taste analyses described above have been restricted to only some of the many components in a taste and/ or smell which give a total experience of the taste or the smell.
  • a method to quantitatively and qualitatively determine the taste or smell of a solid or liquid vegetable or animal oil and fat relies on an analysis of the volatile substances, which are driven off from the oil or fat when heated.
  • the method according to the invention is characterized in that samples of the oil or fat are enclosed in a vial, which vial only to a part is filled with product. The vial and the oil or fat are heated to a predetermined temperature in such a way that the volatile substances are driven off.
  • An adsorbing agent is inserted into the vial, which agent is held in the vial during a predetermined time such that an enrichment of volatile substances on the agent takes place.
  • the agent with adsorbed material is transferred to a gas chromatograph - mass spectrograph (GC-MS) or a gas chromatograph - infrared spectrograph (GC-IR) where the volatile substances are driven off and a spectrum is obtained. This spectrum is compared with spectra for known substances.
  • the method according to the invention is with advantage carried through such that the content of the vial is kept at said predetermined temperature during a time, which is sufficiently long in order to obtain equilibrium between the gas phase and the liquid phase. This is necessary in order to obtain a quantitative analysis of the amount of the taste substances or smell substances, which are present in the oil or fat. If one is interested solely to determine if a certain substance is present or not it is not necessary to wait for an equilibrium condition.
  • the adsorbing agent When the adsorbing agent has been inserted in the vial it is fixed in such a position that it is situated in the gas phase. The adsorbing agent is kept in the vial during 30 - 60 minutes after the equilibrium condition has been achieved.
  • the product in the vial is suitable heated to a temperature of 30-60 °C.
  • the adsorbing agent consists of a quartz glass fiber with a suitable coating.
  • the coating may with advantage consist of a cross- linked polymer.
  • the vials are arranged in the vessel with place for a number of vials.
  • the vessel comprises means, which makes it possible to vary the temperature to which the content of the vials is heated.
  • the vials may be so small that the test volume only is some millimeters or milligrams of the product, which is to be examined.
  • the vial must however in addition to the sample provide space for a gas phase., In the test vial there are also suitably small Teflon coated magnets for stirring.
  • the adsorbent which according to, invention consist of the quartz glass fiber with coating is before inserting into the vial protected by an outer steel needle by means of which, the septum which seals the vial may be penetrated without damaging the fiber.
  • a holder ensures that exactly the same depth is obtained for each sample.
  • the fiber is transferred to a gas chromatograph-mass spectrograph 7 of a suitable kind.
  • the adsorbed substances are desorbed at higlr temperature by a carrying gas.
  • a spectrum is obtained from' the mass spectrograph. This is compared with spectra from known taste Substances or contaminants. This analysis is with advantage carried through using computers.
  • analyses should be sufficiently sensible only fragments of molecules with weights between 30 and 250 amu are registered. Depending on the purpose of the analyses one may concentrate on the presence of a number of cha acteristic substances or on a more complete analysis of all volatile components.
  • the method according to the invention may also be used for sampling in the field. At that it is necessary -to insert the adsorbing agent in a vial in which equilibrium prevails, between the distribution of volatile substances in the liquid and in the respective gas phase above. After a suitable time the adsorbent is removed from the vial and is stored until analysis of the volatile components may take place.

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Seasonings (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

A method for determining taste or smell in liquid or solid vegetable or animal oils and fats, which when heated give off volatile substances comprises enclosing a sample of the product in the vial. The vial is only to a part filled with oil or fat. The oil or fat is heated to a predetermined temperature such that the volatile substances are vaporized. An adsorbing agent is inserted in the vial and is kept in this during a predetermined time such that an enrichment of volatile substances on the agent takes place. The agent with adsorbing material is transferred to a gas chromatograph connected to a mass spectrograph (GC-MS) or a gas chromatograph - infrared spectrograph (GC-IR) where the volatile substances are driven away and a spectrum is obtained. This spectrum is compared with spectra for known taste substances. At that there is obtained a quantitative and qualitative classification of the taste and/or smell of the oil or fat.

Description

Method for determining taste and/or smell in liquid or solid products
The present invention relates to a method for determining taste and/or smell in liquid or solid vegetable or animal oils and fats, which when heated give off volatile substances.
Products where one desires to determine taste and/or smell may consist of different food products in liquid or solid form. For such a determination one uses today often sensory panels, that is persons which have trained their ability to distinguish a certain taste or smell. The experience of a taste or a smell may however be. influenced by different outer circumstances as the form of the day, smoking habits or earlier eaten food. It is also difficult to make an objective comparison between taste or smell experiences made by different test panels.
As example of products where there is a problem to determine the quality of the product using test panels one may mention different animal or vegetable oils or fats.
In the production of animal or vegetable oils the possibility to have a qualitatively and analytical control of taste and smell is of great value. During the production of the oil from oil containing seeds or fruits, the oil is handled in a number of process steps. It is the same when producing oil from an animal material: A bad >or mouldy raw material may result in different funny tastes. A defect in the process as air leaking into the apparatus may give rise to undesirable oxidation products giving off- flavor. An incomplete deodorization may also influence the taste of the oil in a negative manner in that non-desirable compounds are not driven off. Even very small amounts of contaminating components may give rise to an off-odor. It should also be desirable to be able to define a type of taste, specific to a certain kind of oil which may be related to small amounts of specific compounds, which are present in the oil.
Reference is made below to a number of patent documents, which deal with analysis of vegetable oils. These documents have been chosen as example of techniques, which are close to the invention and does not imply that the invention should be limited to analysis of vegetable oils. The method according to the invention may be used on every solid or liquid fat or fatty oil, which when heated gives off volatile substances.
DE 197 58 399 shows how one may use measuring to discover if olive oil or sunflower oil have been- mixed5 with soybean oil, which is done by analyzing different atomic bonds in the oil sample.
DE 43 289 66 describes a method for determining changes in an oil or fat during the time it is used for deep-frying by measuring the ohmic resistance.
In the article "Rapid analysis of vegetable oil flavor quality by dynamic headspace capillary gas chromatography" written by S.K. Raghavan, S.K. Reeder and A. Khyat in Journal of thei American Oil Chemists 'Society 1989, 66 (7) 942-947 there is described determination of the taste quality of vegetable oils. Here one used three compounds in the spectrum that was obtained from the gas chromatograph for comparison between different kinds of oils. The obtained spectrum showed good correspondence to a determination made by a taste panel.
The taste analyses described above have been restricted to only some of the many components in a taste and/ or smell which give a total experience of the taste or the smell. According to the invention there is now proposed a method to quantitatively and qualitatively determine the taste or smell of a solid or liquid vegetable or animal oil and fat. The method relies on an analysis of the volatile substances, which are driven off from the oil or fat when heated. The method according to the invention is characterized in that samples of the oil or fat are enclosed in a vial, which vial only to a part is filled with product. The vial and the oil or fat are heated to a predetermined temperature in such a way that the volatile substances are driven off. An adsorbing agent is inserted into the vial, which agent is held in the vial during a predetermined time such that an enrichment of volatile substances on the agent takes place. The agent with adsorbed material is transferred to a gas chromatograph - mass spectrograph (GC-MS) or a gas chromatograph - infrared spectrograph (GC-IR) where the volatile substances are driven off and a spectrum is obtained. This spectrum is compared with spectra for known substances.
Surprisingly it has been found that it is possible to adsorb the small amounts of taste and/or smell substances driven off from the oil or fat on an agent and later analyse the substances using the spectrograph. By comparing the result with a data library or aroma map for substances usually found in oils and fat, the aroma and/or smell may be secured without uncertain factors. At that there is obtained a quantitative and a qualitative determination of the taste and/ or smell of the product. With the described invention one can obtain a confirmation that the product complies with the demands set for the production process. It is also possible to trace a faulty or contaminated raw material.
The method according to the invention is with advantage carried through such that the content of the vial is kept at said predetermined temperature during a time, which is sufficiently long in order to obtain equilibrium between the gas phase and the liquid phase. This is necessary in order to obtain a quantitative analysis of the amount of the taste substances or smell substances, which are present in the oil or fat. If one is interested solely to determine if a certain substance is present or not it is not necessary to wait for an equilibrium condition.
When the adsorbing agent has been inserted in the vial it is fixed in such a position that it is situated in the gas phase. The adsorbing agent is kept in the vial during 30 - 60 minutes after the equilibrium condition has been achieved.
In order to drive off the volatile components from the product, the product in the vial is suitable heated to a temperature of 30-60 °C.
With advantage the adsorbing agent consists of a quartz glass fiber with a suitable coating. The coating may with advantage consist of a cross- linked polymer.
For the determination of the volatile substances small vials which are sealed with screw cap and septum are used with advantage. The vials are arranged in the vessel with place for a number of vials. The vessel comprises means, which makes it possible to vary the temperature to which the content of the vials is heated. The vials may be so small that the test volume only is some millimeters or milligrams of the product, which is to be examined. The vial must however in addition to the sample provide space for a gas phase., In the test vial there are also suitably small Teflon coated magnets for stirring. The adsorbent which according to, invention consist of the quartz glass fiber with coating is before inserting into the vial protected by an outer steel needle by means of which, the septum which seals the vial may be penetrated without damaging the fiber. A holder ensures that exactly the same depth is obtained for each sample.
Equilibrium between the liquid (or alternatively solid phase) and the gas phase is reached after different times for different products which are to be investigated. In extreme cases several hours may be needed. The distribution coefficient varies in dependence of the temperature and sometimes it may be of advantage tø use a lower temperature and a longer time for adsorptions In many cases a test temperature of 50°C is an optimal compromise. ; In certain, cases such a low temperature as 30°C may be suitable. An optimal adsorption time is in many case 45 minutes after reaching equilibrium.
For the analysis of the adsorbed substances the fiber is transferred to a gas chromatograph-mass spectrograph7 of a suitable kind. The adsorbed substances are desorbed at higlr temperature by a carrying gas. A spectrum is obtained from' the mass spectrograph. This is compared with spectra from known taste Substances or contaminants. This analysis is with advantage carried through using computers.
In order that analyses should be sufficiently sensible only fragments of molecules with weights between 30 and 250 amu are registered. Depending on the purpose of the analyses one may concentrate on the presence of a number of cha acteristic substances or on a more complete analysis of all volatile components.
The method according to the invention may also be used for sampling in the field. At that it is necessary -to insert the adsorbing agent in a vial in which equilibrium prevails, between the distribution of volatile substances in the liquid and in the respective gas phase above. After a suitable time the adsorbent is removed from the vial and is stored until analysis of the volatile components may take place.

Claims

Claims
1. Method for determining taste and/or smell in liquid or solid vegetable or animal oils and fats, which when heated give off volatile substances, characterized in that a sample of the oil or fat is enclosed in a vial, which vial only to a part is filled with oil or fat, after which heating to a predetermined temperature takes place in such a way that the volatile substances are vaporized, that an adsorbing agent is inserted into the vial, which agent is kept in the vial during a predetermined time such that enrichment of volatile substances on the agent takes place, after which the agent with adsorbed material is transferred to gas chromatograph connected to a mass spectrograph (GC-MS) or a gas chromatograph-infrared spectrograph (GC-IR) where the volatile substances are driven away and a spectrum is obtained, which is compared with spectra for known substances, at which there is obtained a quantitative and qualitative determination of the taste and/or smell of product.
2. Method according to claim 1,chanaracterized in that the content in the vial is kept at said predetermined temperature during a time which is sufficiently long in order to obtain equilibrium between gas phase and liquid/solid phase.
3. Method according to claim, 1-2-,< ch a ra racte ri zed in that the adsorbing agent after it has- been inserted in the vial is fixed in such a position that it is situated in the gas phase.
4. Method according to claim 1-3, chararacterized in that the adsorbing agent is kept in the vial during 30-60 minutes after reaching equilibrium.
5. Method according to claim 1-4, chararacterized in that the content in the vial is heated to a temperature of 30-60°C.
6. Method according to claim 1-5, c ha racterized in that the adsorbing agent consists of a quartz glass fiber with a suitable coating.
7. Method according to όlarh Ϊ-B; ! e a racterized in that the coating consists of a cross-linked polymer.
PCT/SE2001/001881 2000-09-05 2001-09-04 Method for determining taste and/or smell in liquid or solid products WO2002021101A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001284587A AU2001284587A1 (en) 2000-09-05 2001-09-04 Method for determining taste and/or smell in liquid or solid products

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE0003147-6 2000-09-05
SE0003147A SE0003147D0 (en) 2000-09-05 2000-09-05 Methods to determine the taste and / or odor of liquid or solid products

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100502954B1 (en) * 2002-08-20 2005-07-25 씨제이 주식회사 Method for measuring the extent of offensive smell in soybean oil
CN104458991A (en) * 2014-12-12 2015-03-25 广东省农业科学院蚕业与农产品加工研究所 Detection method for volatile flavor substance of edible vegetable oil
CN105223065A (en) * 2015-09-16 2016-01-06 上海应用技术学院 The cocktail method for concentration of a kind of blue or green lemon taste

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991015745A1 (en) * 1990-04-02 1991-10-17 Pawliszyn Janusz B Method and device for solid phase microextraction and desorption
WO1999026063A1 (en) * 1997-11-15 1999-05-27 Brechbühler AG Method and equipment for measuring global volatile substances

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991015745A1 (en) * 1990-04-02 1991-10-17 Pawliszyn Janusz B Method and device for solid phase microextraction and desorption
WO1999026063A1 (en) * 1997-11-15 1999-05-27 Brechbühler AG Method and equipment for measuring global volatile substances

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
B. DENIS PAGE ET AL.: "Analysis of volatile contaminants in vegetable oils by headspace solid-phase microextraction with carboxen-based fibres", JOURNAL OF CHROMATOGRAPHY A, vol. 873, 2000, pages 79 - 94, XP002906874 *
HENRYK H. JELEN ET AL.: "Headspace solid-phase microextraction use for the characterization of volatile compounds in vegetable oils of different sensory quality", J. AGRIC. FOOD CHEM., vol. 48, 2000, pages 2360 - 2367, XP002906873 *
S.K. RAGHAVAN ET AL.: "Rapid analysis of vegetable oil flavor quality by dynamic headspace capillary gas chromatography", JAOCS, vol. 66, no. 7, July 1989 (1989-07-01), pages 942 - 947, XP002906875 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100502954B1 (en) * 2002-08-20 2005-07-25 씨제이 주식회사 Method for measuring the extent of offensive smell in soybean oil
CN104458991A (en) * 2014-12-12 2015-03-25 广东省农业科学院蚕业与农产品加工研究所 Detection method for volatile flavor substance of edible vegetable oil
CN105223065A (en) * 2015-09-16 2016-01-06 上海应用技术学院 The cocktail method for concentration of a kind of blue or green lemon taste

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AU2001284587A1 (en) 2002-03-22

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