WO2017093867A1 - Method for determination of total oil/fat content in mayonnaise, royal jelly, and food products containing high amount of emulsifier - Google Patents
Method for determination of total oil/fat content in mayonnaise, royal jelly, and food products containing high amount of emulsifier Download PDFInfo
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- WO2017093867A1 WO2017093867A1 PCT/IB2016/057130 IB2016057130W WO2017093867A1 WO 2017093867 A1 WO2017093867 A1 WO 2017093867A1 IB 2016057130 W IB2016057130 W IB 2016057130W WO 2017093867 A1 WO2017093867 A1 WO 2017093867A1
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- WO
- WIPO (PCT)
- Prior art keywords
- food products
- fat
- products
- methods
- mayonnaise
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 49
- 235000013305 food Nutrition 0.000 title claims abstract description 34
- 229940109850 royal jelly Drugs 0.000 title claims abstract description 22
- 235000010746 mayonnaise Nutrition 0.000 title claims abstract description 19
- 239000008268 mayonnaise Substances 0.000 title claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 12
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003208 petroleum Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims 5
- 235000013599 spices Nutrition 0.000 claims 2
- 235000013311 vegetables Nutrition 0.000 claims 2
- 238000000605 extraction Methods 0.000 abstract description 10
- 229930014626 natural product Natural products 0.000 abstract description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 235000013365 dairy product Nutrition 0.000 abstract description 3
- 235000013372 meat Nutrition 0.000 abstract description 3
- 235000013622 meat product Nutrition 0.000 abstract description 3
- 238000000944 Soxhlet extraction Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 8
- 239000000049 pigment Substances 0.000 description 7
- 239000000284 extract Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000012454 non-polar solvent Substances 0.000 description 4
- 239000001993 wax Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 235000013861 fat-free Nutrition 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000011877 solvent mixture Substances 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 235000021149 fatty food Nutrition 0.000 description 1
- 239000000576 food coloring agent Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000021067 refined food Nutrition 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000021055 solid food Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- G01N33/04—Dairy products
- G01N33/06—Determining fat content, e.g. by butyrometer
-
- 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
-
- 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
- G01N33/025—Fruits or vegetables
-
- 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
Definitions
- TECHNICAL FIELD The invention covers the industry, research institutions, universities and private sector testing /analysis laboratory operating in the field of food industry.
- the present disclosure contributes to food sector study in the determination of total oil/fat content and fatty food product formulation (especially high amount emulsifier contain foodstuffs, mayonnaise, and royal jelly).
- PREVIOUS TECHNIQUE The invention covers the industry, research institutions, universities and private sector testing /analysis laboratory operating in the field of food industry.
- the present disclosure contributes to food sector study in the determination of total oil/fat content and fatty food product formulation (especially high amount emulsifier contain foodstuffs, mayonnaise, and royal jelly).
- the aim of the present invention is to improve the existing methods for the determination of total oil/fat content in foodstuffs and provide a solution for current methods (standard and patented methods) that have technical problems in some food matrices. Therefore, a new method was developed by improving the sample preparation and extraction procedures of the commonly used current methods. Although this method has been developed for the determination of fat/oil content in food matrices which the current methods are not applicable or inappropriate, it can be used safely for in determination of total fat/oil content of general foodstuff.
- Non-polar solvents soluble waxes, some pigments or food colorants, some non-fat/oil components extract with fat/oil during extraction cannot be separated from the fat/oil with regular common methods. This affected the real value of the fat/oil content of the food products.
- absorbent such as silica gel 60.
- silica gel 60 adsorbed waxes, pigments etc. not allowed to go solvent extract together with oil/fat. So that the extracts obtain from soxhlet is fat or oil without pigments, wax, and other non-polar solvent soluble. Results obtained from soxhlet extract express the real value of the fat or oil content in food products.
- i-) mayonnaise and royal jelly ii-) high amount emulsifier content food products
- iii-) natural products contain pigments or colorants and not fat/oil component that soluble in solvent use for oil/fat content determination
- Silica gel 60 was added via spatula slowly to the beaker containing royal jelly and sea sand and mixture is homogenized.
- Soxhlet cartridge is charged 1 cm height with silica gel 60.
- the mixture is added into the soxhlet cartridge with 1 cm height silica gel 60 and covered with fat free cotton.
- Cartridge is put into soxhlet apparatus.
- Fat recovery flask was weighed (M 2 ).
- Recovery flask is put into desiccator, cooled to room temperature and weighed (M 3 ).
- Total fat is calculated by the formula:
- M-i amount of sample M 2 : Weight of recovery flask M 3 : Fat + weight of recovery flask M 4 : amount of moisture M 5 : 100 - M 4 (amount of dry matter) b-) Mayonnaise samples
- the melting point of given compound is below than 80 ⁇ C, the sample is melted. Then, the detailed experimental procedure and calculation formula is applied for the total fat determination.
- the food products having the melting point higher than 80 ⁇ C are acid hydrolysed according to the regular methods (ISO, AOCS, lUPAC etc.). Briefly, 20 mL 4 N HCI is poured into 10 g of sample, and heated to hydrolyse. After hydrolysis, sample is cooled to room temperature and 20 mL distilled water is added, filtrated through filter paper and dried in oven at 105 ⁇ C. The detailed expe rimental procedure and calculations of mayonnaise and royal jelly are applied to the sample which is hydrolysed according to regular methods.
- Natural samples first extracted with nonpolar solvent and then the extract is adsorbed on silica gel 60. Then, it is extracted in soxhiet apparatus and total fat amount is determined. Total fat determination procedure is explained as;
- homogenization is performed by grinder or mixer.
- Powder sample is added into the cartridge that contains 1 cm height silica gel 60 and covered with oil free cotton, then extracted for 2 hours.
- the invention is used as a fat/oil determination method for the identification of total fat/oil content in food products by the related laboratories and industries.
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- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Seasonings (AREA)
Abstract
There are many common methods used for determination of fat/oil content in food products. Depending on the product type acid hydrolysis with soxhlet extraction, direct soxhlet (without acid hydrolysis) extraction or Gerber techniques are used in such kinds of the ordinary methods. Some of the methods rapidly identified total fat/oil content in food products with analytical instruments. These common methods cover determination of fat/oil content of meat and meat products, processed foodstuffs, dairy products and oily natural products. In the study, we underline that existing methods are not suitable or have some problems with some kinds of foodstuffs. Thus, new alternative methods are required to determine fat/oil content in such kinds of problematic food products (mayonnaise, royal jelly, food products containing high amount of emulsifiers and natural products). Improved method provides a novelty in sample preparation and extraction steps which are problematic with ordinary methods.
Description
DESCRIPTION
METHOD FOR DETERMINATION OF TOTAL OIL/FAT CONTENT IN
MAYONNAISE, ROYAL JELLY, AND FOOD PRODUCTS CONTAINING HIGH
AMOUNT OF EMULSIFIER
TECHNICAL FIELD The invention covers the industry, research institutions, universities and private sector testing /analysis laboratory operating in the field of food industry. The present disclosure contributes to food sector study in the determination of total oil/fat content and fatty food product formulation (especially high amount emulsifier contain foodstuffs, mayonnaise, and royal jelly). PREVIOUS TECHNIQUE
There are many studies in the literature about the total fat/oil determination. Although most of these studies are similar, some of them contain novelty. Many of them are common standard methods (such as ISO, AOCS, AOAC, lUPAC, TSE etc.) or compilation of these methods. In the literature, patents related to the determination of total oil/fat in foodstuffs are about development or modification of the devices. There are also available patents in the literature related to solvents and solvent mixtures used for extraction of fat or oil from food products for the determination of total oil/fat content. Many of these patents have been improved by the modifications of the known reference standard methods (such as ISO, AOCS, AOAC etc.).
In this study, the aim of the present invention is to improve the existing methods for the determination of total oil/fat content in foodstuffs and provide a solution for current methods (standard and patented methods) that have technical problems in some food matrices. Therefore, a new method was developed by improving the sample preparation and extraction procedures of the commonly used current methods. Although this method has been developed for the determination of fat/oil content in food matrices which the current methods are not applicable or inappropriate, it can be used safely for in determination of total fat/oil content of general foodstuff.
TECHNICAL SOLUTION
Ordinary analysis methods cannot determine exact value of oil/fat content in mayonnaise, royal jelly and other food products containing high amount of emulsifiers. There are many methods in the literature relate to the determination of total fat/oil content in food products. Generally, these methods/or procedures are designed to determine fat/oil content of meat and meat products, processed foods, dairy products and unprocessed food products. In the present work, we emphasize that current methods are not appropriate for some types of food products. It is, therefore, an object of the present invention to provide an alternative method for determining precise values of fat/oil contents of inappropriate food samples with current methods.
DETAILED DESCRIPTION OF THE METHOD
There are many usual methods used for detection of total fat/oil content in foodstuffs. Depending on the product type acid hydrolysis with soxhlet extraction, direct soxhlet (without acid hydrolysis) extraction or Gerber techniques are used in such kinds of the ordinary methods. Some of the methods rapidly identified total fat/oil content in food products with analytical instruments. Generally these common methods use for meat and meat products, processed foodstuffs, dairy products, and oily natural products (such as oily seeds). In the study, we underline that existing methods are not suitable for extraction of oil/fat from mayonnaise, royal jelly and high amount emulsifier food products. As the sample preparation and extraction steps of these methods is insufficient for such kinds of food products. Therefore in this study, the sample preparation and extraction steps of the mayonnaise, royal jelly, other food products containing high amount of emulsifiers and non-polar solvent soluble pigment containing natural products ( such as wax, pigments etc.) products were improved.
Non-polar solvents soluble waxes, some pigments or food colorants, some non-fat/oil components extract with fat/oil during extraction cannot be separated from the fat/oil with regular common methods. This affected the real value of the fat/oil content of the food products. We have solved these problems in our methods using absorbent such as silica gel 60. In the method condition silica gel 60 adsorbed waxes, pigments etc. not allowed to go solvent extract together with oil/fat. So that the extracts obtain from soxhlet is fat or oil without pigments, wax, and other non-polar solvent soluble.
Results obtained from soxhlet extract express the real value of the fat or oil content in food products.
Three different types of food products are studied. These are i-) mayonnaise and royal jelly, ii-) high amount emulsifier content food products, iii-) natural products (contain pigments or colorants and not fat/oil component that soluble in solvent use for oil/fat content determination), respectively. i-) Mayonnaise and royal jelly products
In mayonnaise and royal jelly studies, sample is adsorbed on silica gel 60 and transformed into dust particles. Then, sample is extracted with appropriate solvents. Experimental procedure detail and calculation is indicated as: a-) Royal jelly samples
1 0 g of royal jelly is weighed into beaker (M-i) and 1 g of sea sand is added.
Silica gel 60 was added via spatula slowly to the beaker containing royal jelly and sea sand and mixture is homogenized.
Soxhlet cartridge is charged 1 cm height with silica gel 60.
The mixture is added into the soxhlet cartridge with 1 cm height silica gel 60 and covered with fat free cotton.
Cartridge is put into soxhlet apparatus.
Fat recovery flask was weighed (M2).
Using an appropriate amount of petrol ethenhexane (80:20) depending on recovery flask, sample is extracted for three hours at 1 50<C.
Solvent was removed from recovery flask.
Recovery flask is put into desiccator, cooled to room temperature and weighed (M3).
• If the moisture amount of royal jelly is not definite, percent moisture amount is calculated (M4).
Total fat is calculated by the formula:
Total fat content of dry matter is calculated as:
Total fat = [( 3 - M2) ÷ M2 X 100] X (100 ÷ MS)
M-i : amount of sample M2: Weight of recovery flask M3: Fat + weight of recovery flask M4: amount of moisture M5: 100 - M4 (amount of dry matter) b-) Mayonnaise samples
The route and calculations applied for royal jelly samples are used for mayonnaise samples.
M-) Food products containing high amount of emulsifier
Food products containing high amount of emulsifier are adsorbed on silicagel 60 directly, melted or hydrolyzed depending on physical characteristics, and turned into powder. Then, it is extracted with an appropriate solvent. Experimental procedure is explained as; a-) Total fat procedure of gel structure food products
Experimental procedure and calculations stated for royal jelly and mayonnaise products are applied. However; petroleum ether:hexane:acetone (80:15:5) is used as solvent mixture, extraction time is 4 hours and temperature is 150<C. b-) Total fat procedure of solid food products
If the melting point of given compound is below than 80<C, the sample is melted. Then, the detailed experimental procedure and calculation formula is applied for the total fat determination.
The food products having the melting point higher than 80<C, are acid hydrolysed according to the regular methods (ISO, AOCS, lUPAC etc.). Briefly, 20 mL 4 N HCI is poured into 10 g of sample, and heated to hydrolyse. After hydrolysis, sample is cooled to room temperature and 20 mL distilled water is added, filtrated through filter paper and dried in oven at 105<C. The detailed expe rimental procedure and
calculations of mayonnaise and royal jelly are applied to the sample which is hydrolysed according to regular methods.
Mi-) Pigment, colorants, and natural samples including nonpolar extract except fat
Natural samples first extracted with nonpolar solvent and then the extract is adsorbed on silica gel 60. Then, it is extracted in soxhiet apparatus and total fat amount is determined. Total fat determination procedure is explained as;
• Depending on type of sample, homogenization is performed by grinder or mixer.
· 10 g (M-i) of homogenized sample is weighed into soxhiet cartridge.
• Sample is extracted by diethyl ether at I SO'C for 3 hours (petroleum ether or hexane could be used).
• Petroleum ether is evaporated, and extracted is dissolved in minimum amount of dichloromethane.
· Silica gel 60 is added slowly and sample is transformed into powder.
• Powder sample is added into the cartridge that contains 1 cm height silica gel 60 and covered with oil free cotton, then extracted for 2 hours.
• Solvent is removed from the recovery flask weight of which is known (M2).
• Recovery flask is put into desiccator, cooled to room temperature and weighed (M3).
• If total fat in dry matter is asked, moisture percentage should be calculated (M4).
• Total fat amount is calculated according to the formula for royal jelly and mayonnaise. APPLICATION OF THE INVENTION IN INDUSTRY
The invention is used as a fat/oil determination method for the identification of total fat/oil content in food products by the related laboratories and industries.
Claims
1 . A method for total fat/oil determination in food products via soxhiet apparatus, comprising the use of silica gel 60 as adsorbent for determination of total fat/oil in
- Mayonnaise and mayonnaise containing products
- Royal jelly and royal jelly containing products
- Food products containing high amount of emulsifier
- Natural food products (oil seeds, vegetables, spices etc.)
2. A method according to claim 1 wherein, for mayonnaise and mayonnaise containing products silica gel 60 as adsorbent, petroleum ethenhexane (80:20) as solvent is used and temperature is set to 150<C.
3. A method according to claim 1 wherein, for royal jelly and royal jelly containing products silica gel 60 as adsorbent, petroleum ethenhexane (80:20) as solvent is used and temperature is set to 150<C.
4. A method according to claim 1 wherein, for foods products containing high amount of emulsifier silica gel 60 as adsorbent, petroleum ether:hexane:acetone (80:15:5) as solvent is used and temperature is set to 150*0.
5. A method according to claim 1 wherein, for natural food products (oil seeds, vegetables, spices etc.) silica gel 60 as adsorbent, petroleum ether as solvent is used and temperature is set to 130<C.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TRTR2015/15233 | 2015-12-01 | ||
| TR201515233 | 2015-12-01 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2017093867A1 true WO2017093867A1 (en) | 2017-06-08 |
Family
ID=57915017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/IB2016/057130 WO2017093867A1 (en) | 2015-12-01 | 2016-11-25 | Method for determination of total oil/fat content in mayonnaise, royal jelly, and food products containing high amount of emulsifier |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2017093867A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12274280B2 (en) * | 2023-07-27 | 2025-04-15 | Henan Zhongda Hengyuan Biotechnology Stock Co., Ltd. | Method for extracting oils from sauces while simultaneously determining fat content, peroxide value, and acid value |
-
2016
- 2016-11-25 WO PCT/IB2016/057130 patent/WO2017093867A1/en active Application Filing
Non-Patent Citations (2)
| Title |
|---|
| GUNAWAN ET AL: "Separation and purification of squalene from soybean oil deodorizer distillate", SEPARATION AND PURIFICATION TECHNOLOGY, ELSEVIER SCIENCE, AMSTERDAM, NL, vol. 60, no. 2, 19 March 2008 (2008-03-19), pages 128 - 135, XP022542863, ISSN: 1383-5866, DOI: 10.1016/J.SEPPUR.2007.08.001 * |
| SUBRAMANIAN R ET AL: "Double bypasses soxhlet apparatus for extraction of piperine fromPiper nigrum", ARABIAN JOURNAL OF CHEMISTRY, SAUDI CHEMICAL SOCIETY, SA, vol. 9, 25 June 2011 (2011-06-25), XP029786907, ISSN: 1878-5352, DOI: 10.1016/J.ARABJC.2011.06.022 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12274280B2 (en) * | 2023-07-27 | 2025-04-15 | Henan Zhongda Hengyuan Biotechnology Stock Co., Ltd. | Method for extracting oils from sauces while simultaneously determining fat content, peroxide value, and acid value |
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