KR20170045514A - Filtration method to reduce benzo(a)pyrene contents by minimizing reduction of volatiles in sesame oil - Google Patents
Filtration method to reduce benzo(a)pyrene contents by minimizing reduction of volatiles in sesame oil Download PDFInfo
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- KR20170045514A KR20170045514A KR1020150145155A KR20150145155A KR20170045514A KR 20170045514 A KR20170045514 A KR 20170045514A KR 1020150145155 A KR1020150145155 A KR 1020150145155A KR 20150145155 A KR20150145155 A KR 20150145155A KR 20170045514 A KR20170045514 A KR 20170045514A
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- activated carbon
- compressed oil
- sesame oil
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- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 title claims abstract description 33
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 title abstract description 6
- 239000008159 sesame oil Substances 0.000 title description 28
- 235000011803 sesame oil Nutrition 0.000 title description 28
- 238000001914 filtration Methods 0.000 title description 4
- 239000003039 volatile agent Substances 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 105
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 17
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims description 18
- 239000011148 porous material Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000002304 perfume Substances 0.000 claims description 5
- 241000207961 Sesamum Species 0.000 claims description 3
- 235000003434 Sesamum indicum Nutrition 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 abstract description 15
- 239000000796 flavoring agent Substances 0.000 abstract description 6
- 235000019634 flavors Nutrition 0.000 abstract description 6
- 238000004321 preservation Methods 0.000 abstract description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 27
- 239000003921 oil Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 15
- 238000013019 agitation Methods 0.000 description 11
- KYNSBQPICQTCGU-UHFFFAOYSA-N Benzopyrane Chemical compound C1=CC=C2C=CCOC2=C1 KYNSBQPICQTCGU-UHFFFAOYSA-N 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
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- 235000013305 food Nutrition 0.000 description 8
- 230000001603 reducing effect Effects 0.000 description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001994 activation Methods 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
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- FMMWHPNWAFZXNH-AQZSQYOVSA-N 1,2,3,4,5,6,7,8,9,10,11,12-dodecadeuteriobenzo[a]pyrene Chemical compound [2H]C1=C2C3=C([2H])C([2H])=C([2H])C([2H])=C3C([2H])=C(C([2H])=C3[2H])C2=C2C3=C([2H])C([2H])=C([2H])C2=C1[2H] FMMWHPNWAFZXNH-AQZSQYOVSA-N 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 238000003775 Density Functional Theory Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- WHQSYGRFZMUQGQ-UHFFFAOYSA-N n,n-dimethylformamide;hydrate Chemical compound O.CN(C)C=O WHQSYGRFZMUQGQ-UHFFFAOYSA-N 0.000 description 2
- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- -1 polydimethylsiloxane Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- 239000012925 reference material Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
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- 244000061176 Nicotiana tabacum Species 0.000 description 1
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- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 235000019568 aromas Nutrition 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
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- 239000012159 carrier gas Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
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- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- IYWCBYFJFZCCGV-UHFFFAOYSA-N formamide;hydrate Chemical compound O.NC=O IYWCBYFJFZCCGV-UHFFFAOYSA-N 0.000 description 1
- 231100000025 genetic toxicology Toxicity 0.000 description 1
- 230000001738 genotoxic effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 231100000003 human carcinogen Toxicity 0.000 description 1
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- 239000010422 internal standard material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000010461 other edible oil Substances 0.000 description 1
- 239000003415 peat Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
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- 150000003216 pyrazines Chemical class 0.000 description 1
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- 239000000779 smoke Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
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- 239000002023 wood Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B9/00—Presses specially adapted for particular purposes
- B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
-
- C01B31/08—
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2250/00—Food ingredients
- A23V2250/20—Natural extracts
- A23V2250/21—Plant extracts
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/02—Adsorption
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2300/00—Processes
- A23V2300/16—Extrusion
Abstract
The present invention relates to a compressed oil production method for simultaneously achieving reduction in benzo (a) pyrene and preservation of fragrance components, wherein activated carbon having certain requirements is added to the raw material compressed oil and stirred under a predetermined condition to reduce benzopyrene And pyrazine flavor component preservation can be achieved at the same time.
Description
The present invention relates to a compressed oil production method for simultaneously achieving reduction of benzo (a) pyrene and preservation of fragrance components.
Sesame oil is a favorite food in Korea and Asia to give traditionally delicious flavors and aromas. In Korea, sesame oil is processed by high temperature roasting and squeezing to improve flavor and aroma when making sesame oil. Compared with other edible oils, pressed sesame oil is processed by simple precipitation separation, filtration , It is often the case that the raw material itself remains in the final product when it is contaminated.
In particular, polycyclic aromatic hydrocarbons (PAHs), which can be generated during the production of sesame oil, are organic compounds in which two or more aromatic rings are fused and can appear in the combustion process of carbohydrates such as sesame. Some PAHs, such as a) pyrene, are known to exhibit genotoxicity and carcinogenicity, and these substances remain a problem in sesame oil.
Benzo (a) pyrene is a yellow crystalline solid belonging to the polycyclic aromatic hydrocarbons (PAHs) group, and is produced by incomplete combustion at temperatures between 300 and 600 ° C. It is present mainly in coal tar, car exhaust gas (especially diesel engine), tobacco smoke, and also in foods that have not been cooked / processed such as agricultural products, fish and shellfish due to environmental pollution and carbohydrates and proteins , Lipids, etc. are also decomposed. Benzopyran is a long-term and potentially toxic substance. It is an endocrine disrupting substance and carcinogenic substance. It is a priority list for the risk assessment of CODEX and JECFA (Joint FAO / WHO Food Additives Committee) And is becoming a subject of global interest. The International Agency for Research on Cancer (IARC) recently upgraded benzopyran to a human carcinogen in
The regulation of benzoprene produced in edible oil production process is controlled by 2.0 ppb of EU, 5.0 ppb of Spain and 10 ppb of China, and recommended specification is set to 2.0 ppb or less in accordance with the most strictly regulated EU standards in Korea. .
In order to reduce the harmfulness of benzopyran, various biological, physical / chemical methods have been proposed. In particular, the method of reducing benzopyrene produced in edible oil in foods has been proposed, for example, .
Conventional methods for reducing benzopyrene in edible oils include absorbing edible oil in clay, carbonizing the absorbed edible oil and activating the carbon to use acid-activated clay as an absorbent (US Pat. No. 5,218,132). The carbonization and activation step of the edible oil in this method is performed by heating in the presence of zinc chloride, which is an active agent, and the activation temperature should be 250 ° C. or higher.
However, this method can be applied to general edible oil, but in case of pressed oil, especially sesame oil, flavor and color may change due to clay or temperature.
On the other hand, active carbon is a special carbon that is calcined and renewed at high temperature by using coconut shell, wood, coal, etc. as a raw material. It is a collection of amorphous carbon with fine pores of molecular size well developed during activation process. Manufacture raw materials can be divided into food materials, animal matter, minerals, industrial wastes and so on. In the case of minerals, coal and petroleum can be distinguished. In general, powdered activated carbon is produced using a raw material of a food material, and charcoal, coconut shell, coal and the like are used for producing granular activated carbon. Activated carbon has been studied and utilized in various fields due to its properties such as adsorption.
Although there have been studies on the use of activated carbon in the food manufacturing process due to the nature of activated carbon, there has been no research on optimal activated carbon and process conditions for reducing benzopyrene and maintaining the fragrance components. There was a need for research.
Accordingly, the present inventors have completed the present invention by establishing an optimal activated carbon condition and a sesame oil manufacturing process which reduce the benzopyrene content of sesame oil and maintain the quality of sesame oil while preserving aroma components.
An object of the present invention is to provide an optimum compressed oil production method for reducing benzopyrene and preserving a perfume component.
In order to achieve the above object,
1) preparing raw material compressed oil through roasting and pressing process from raw material;
2) a step of adding activated carbon to the compressed oil of step 1) followed by stirring, wherein the benzopyrene is reduced, and a compressed oil is preserved in which a perfume component is preserved.
According to the production method of the present invention, benzoprene which can occur in the production of compressed oil can be effectively removed, and the inherent flavor of the compressed oil can be preserved. Therefore, safety can be secured and inherent quality can be maintained can do.
1 is a graph showing cumulative surface area for each activated carbon sample.
FIG. 2 is a graph showing the cumulative pore volume for each activated carbon sample (nm is a unit for diameter).
FIG. 3 is a graph showing the total pore surface area for each activated carbon sample.
FIG. 4 is a view showing the surface area of a mesopore for each activated carbon sample.
5 is a graph showing the surface area of micropore for each activated carbon sample.
FIG. 6 is a view showing the contents of pyrazine components after adding each activated carbon sample to sesame oil. FIG.
FIG. 7 is a view showing the content ratio of carbon / oxygen (C / O) in each activated carbon sample.
8 is a graph showing changes in content of pyrazine aroma components with stirring speed.
FIG. 9 is a graph showing the results of analyzing the content of benzopyrene after adding each activated carbon sample to sesame oil, and the graph on the right side shows the surface area of the pores having a pore size of 1.7 nm to 10.0 nm and the carbon / oxygen content Fig.
FIG. 10 is a graph showing the content of benzopyran component according to the stirring speed of FIG. 10. FIG.
Hereinafter, the present invention will be described in detail.
The present invention
1) preparing raw material compressed oil through roasting and pressing process from raw material;
2) a step of adding activated carbon to the compressed oil of step 1) followed by stirring, wherein the benzopyrene is reduced, and a compressed oil is preserved in which a perfume component is preserved.
The raw material of the step 1) may be sesame but is not limited thereto.
The activated carbon in step 2) is preferably used in an amount of 0.3 part by weight to 1 part by weight based on the weight of raw material compressed in step 1), but is not limited thereto. The total surface area of pores having a diameter of 1.7 nm to 10.0 nm is 250 m 2 / g to 450 m 2 / g, but is not limited thereto, and the carbon / oxygen content ratio may be 5.5 to 9, but is not limited thereto.
The stirring of step 2) may be performed at 400 rpm to 800 rpm for 5 minutes to 60 minutes, and most preferably at 600 rpm for 40 minutes to 45 minutes. However, the perfume component of step 3) But is not limited to, pyrazine components.
According to a preferred embodiment of the present invention, in order to find an optimum condition for maintaining a fragrance component while reducing benzopyran in a compressed oil, the present inventors purchased five kinds of activated carbon having different pore distributions and analyzed the pores, The addition of each of the five kinds of activated carbon to the oil and stirring at a constant rpm confirmed that the pyrazine fragrance component can be more effectively preserved and the benzoprene can be reduced at the same time as described above.
If the amount of activated carbon is less than 0.3 parts by weight based on the raw material compressed oil, the benzoprene reduction effect is low. If the amount of activated carbon is more than 1 part by weight, benzoprene can be reduced but it is difficult to preserve the quality of compressed oil. To 1 part by weight, and it is most preferable to use 0.5 part by weight. In addition, when the total surface area of 1.7 nm to 10 nm size pores of diameter of the activated carbon is less than 250 m 2 / g when lack the benzopyrene reducing effect exceeds 450 m 2 / g lowers the quality such as flavor components 250 m 2 / g To 450 m < 2 > / g is preferable, and it is preferable that the carbon / oxygen content ratio is preferably 5.5 to 9 and more preferably 6 to 9. [
If the agitation of the step 2) is less than 5 minutes, the effect of agitation is insufficient. When the agitation exceeds 60 minutes, there is a fear that the preservation of the quality such as the fragrance ingredient may be hindered. It is preferable to perform the agitation for 5 minutes to 60 minutes, According to the aspect of the present invention, it was found that the fragrance component can be effectively preserved and the benzopyrene can be effectively reduced for 40 to 45 minutes. If the agitation speed is less than 400 rpm, the effect of agitation is insufficient. If the agitation speed exceeds 800 rpm, there is a possibility that the equipment cost and practicality may be lowered. It is preferable that the agitation speed is 400 rpm to 800 rpm. According to the aspect, it was confirmed that when the mixture was stirred at 600 rpm for 40 minutes to 45 minutes, the fragrance ingredient could be effectively preserved and the benzopyrene could be reduced.
Hereinafter, embodiments and experimental examples of the present invention will be described in detail.
It is to be understood, however, that the following examples and experimental examples are illustrative of the present invention and that the present invention is not limited by the following examples and experimental examples.
< Example 1> Pore analysis of activated carbon
Five kinds of activated carbon for use in the filtration of sesame oil were purchased from the market to produce overall pores, mesopores (mesopores between 20 Å and 500 Å) and micropores (mesopores with a size of less than 20 Å) Respectively.
First, the activated carbon is a mixture of powdered activated carbon (SGC-PW, Shin Kwang Chemical Industry, Korea), granular activated carbon (SGC-GW, Shin Kwang Chemical Ind., Korea), powdered activated carbon (SGC- Powder activated carbon (OSC-P, Osung Company, Korea) using granular activated carbon (SAM-GC, Samchully, Korea) and peat as raw materials was used. The surface area of the activated carbon pores is measured by the Autosorb-iQ 2ST / MP (Brunauer-Emmett-Teller equation) using the so-called BET equation (Brunauer-Emmett-Teller equation) in which the surface area is calculated by measuring the volume of the monolayer when the nitrogen is physically adsorbed on the activated carbon surface at a constant temperature Quantachrome, florida, USA). As a result, the cumulative surface area of SGC-PC and SGC-PW was high as shown in FIG. 1 (FIG. 1). As a result of analyzing the distribution of pores using this, the cumulative pore volume of SGC-PW and SGC-GW was high as shown in FIG. 2 (FIG. 2).
Mesoporous mesopores can be estimated by surface adsorption using a known nitrogen adsorption and mercury porosimetry technique. In the present invention, the so-called Barrett- The micropore was analyzed by density functional theory (DFT). The results are shown in FIG. 3, FIG. 4, and FIG. 5, SGC-PC and SGC-PW showed high surface area (Fig. 3), and SGC-PW and SGC-GW were high in mesopore (Fig. 4) -GW (Fig. 5).
< Experimental Example 1> Addition of activated carbon and In agitation Following Pyrazine species Analysis of content of fragrance ingredient
The five kinds of activated carbons disclosed in Example 1 were added to sesame oil, respectively, and chromaticity and residual aroma components were analyzed.
Specifically, after purchasing sesame oil (pure Jimmy's famous sesame oil, Cheongyang food, Korea) sold on the market, the sesame oil samples were divided into five groups, and the five kinds of activated charcoal described in Example 1 were added to sesame oil 0.5% based on the weight of the sample.
<1-1> Pyrazine species Fragrance component analysis
To analyze pyrazine fragrance components, aroma components were extracted using solid phase microextraction (SPME) method. The SPME fiber used was 50/30 ㎛ divinylbenzene / carboxen / polydimethylsiloxane (DVB / CAR / PDMS) fiber (Supleco, Bellefonte, PA, USA) and 20 mL of sesame oil was placed in a 50 mL brown vial. septum (Supleco, Bellefonte, Pa., USA). The specific analysis conditions of the SPME method are shown in Table 1.
In order to analyze the fragrance components extracted by the above method, GC-MS (Gas Chromatograph-Mass spectrophotometry) was performed. The instrument was equipped with a mass selective detector (model 5975C, Agilent Technologies, Palo Alto, Calif., USA) on a model 6890A (Agilent Technologies, Palo Alto, The conditions of the GC-MS used in the experiment are shown in Table 2.
For quantitative analysis, 0.3 mL of p-cymene was dissolved in 1,000 ppm (w / v, in paraffin oil) using an internal standard (GC-MS Wiley7 library, Agilent Technologies, Palo Alto, CA, USA) Materials (internal standard, IS) were used in the sample. Quantitative values were calculated by GC / MS total ion chromatogram as peak area of compound / peak area of I.S. In order to analyze the effect of distributed elements in activated carbon, distribution elements were identified using Multilab ESCA 2000 (VG Microtech, Korea). As a result, the residual total amount of the pyrazine components for each type of activated carbon was as shown in FIG. 6, and it was confirmed that the reduction amount varied depending on the total volume of the pores and the carbon / oxygen content ratio of the activated carbon 7).
<1-2> On stirring speed Following Pyrazine Fragrance ingredient preservation analysis
In order to confirm the stirring speed for preventing the loss of the fragrance component of pyrazine, the content of pyrazine fragrance component was analyzed according to the stirring speed after addition of activated carbon.
Specifically, activated carbon SGC-PW was added to the sesame oil sample, and the stirring conditions (temperature and time conditions are the same) were set to 200 rpm, 400 rpm and 600 rpm, respectively, in the SPME method of Experimental Example <1-1> The content of pyrazines was analyzed in the same manner as in GC-MS of Experimental Example <1-1>. As a result, as shown in FIG. 8, when the rpm was 600 as compared with 200 or 400, Was found to be the highest, and it was confirmed that the higher the stirring rotation number, the better the preservation of aroma.
< Experimental Example 2> Addition of activated carbon and In agitation Of benzopyran ( Benzo (a) pyrene ) Content analysis
The five kinds of activated carbons described in the above <Example 1> were added to sesame oil and stirred, respectively, and the content of benzopyrene was analyzed.
<2-1> Sample preparation
In order to increase the benzopyrene content of the sesame oil sample of Experimental Example 1, sesame oil containing 10 ppm benzopyran was prepared and diluted 1/200 times to make a final concentration of 500 ppb (w / w) benzopyran-containing sesame oil (1,000 g) Then, sesame oil (3.000 g) containing 5 ppb (w / w) benzopyran was prepared by diluting with 1/100 times, and then left at room temperature for one day or more. Benzo (a) pyrene was 99% pure (Supleco, Bellefonte, PA, USA) and the solvent was HPLC grade water and methanol (J.T Baker, Phillipsburg, NJ, USA).
<2-2> Preparation of Test Solution
Benzo (a) pyrene was used as the reference material, Benzo (a) pyrene-d12 was used as the internal standard, and liquid / liquid extraction method was used as the pretreatment method.
Specifically, 200 μL of Benzo (a) pyrene-d12 was added to 10 g of the sample prepared in Experimental Example <2-1>, dissolved in 100 mL of hexane, transferred to the separating funnel (I), and N, N-
In addition, silica cartridges were preliminarily activated by discharging dichloromethane (10 mL) and hexane (20 mL) at a rate of 2 ~ 3 drops per second for purification. The concentrate was added to the cartridge at a rate of 1 mL / min, followed by sequential elution with 5 mL of hexane and 15 mL of a mixture of hexane / dichloromethane (3: 1). The eluate was concentrated at 40 ° C under nitrogen The residue was dissolved in dichloromethane to make a total volume of 200 μL, which was then filtered through a 0.45 μm membrane filter to purify the test solution.
<2-3> Measurement of benzopyran content
The test solution according to the above Experimental Example <2-2> was separately prepared before and after the addition of active carbon and stirring, and the content of benzopyrene was measured by GC-MS.
As the analysis condition of GC-MSD, the column was HP-5MS U.I. The oven temperature was maintained at 100 ° C for 10 minutes, then increased to 280 ° C at a rate of 60 ° C / minute, and the temperature was maintained for 10 minutes. The column was kept at 30 ° C / min Post-run at 310 ° C for 10 minutes. Helium gas was flowed at 1.5 ml / min as a carrier gas. At this time, GC inlet temperature was 320 ° C, ionization energy was 70 eV, and 1 μL sample was injected in splitless mode. The parameters are shown in Table 3.
A calibration curve was prepared with the area ratio [A S / A IS ] of the standard material and the internal standard material obtained from the calibration curve standard solution as the Y axis and the standard substance concentration as the X axis, and the peak area ratio [A SAM / A SAMIS ] was assigned to the Y axis to calculate the concentration of benzopyrene:
A S : Standard peak area of the calibration curve standard solution;
A IS : internal reference material peak area of the calibration curve standard solution;
A SAM : 4 PAHs peak area of test solution; And
A SAMIS : Peak area of internal standard material of test solution.
As a result, it was confirmed that the benzopyrene was reduced according to the total surface area of micropores having a diameter of 1.7 nm to 10.0 nm in diameter of the activated carbon and the carbon / oxygen content ratio of the activated carbon (FIG. 9).
In order to confirm the degree of reduction of benzopyrone according to the stirring speed, the agitation speed rpm was set to 200, 400, and 600, respectively, for the sample to which SGC-PW activated carbon was added. The benzopyrene content was analyzed and compared with the control group without active carbon addition and agitation, it was confirmed that the higher the rpm, the more the benzopyrene content was reduced (FIG. 10).
Claims (8)
2) a step of adding activated carbon to the compressed oil of step 1) and then stirring the reduced activated carbon, wherein the benzopyrene is reduced and the perfume component is preserved.
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| CN107283895A (en) * | 2017-06-14 | 2017-10-24 | 郑州永泰澳新商贸有限公司 | A kind of Domestic oil press for integrating frying, crushing and squeezing |
| KR102437589B1 (en) * | 2021-11-19 | 2022-08-29 | 경기도 | Method of Manufacturing Perilla Oil with Reduced Specific Odor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107283895A (en) * | 2017-06-14 | 2017-10-24 | 郑州永泰澳新商贸有限公司 | A kind of Domestic oil press for integrating frying, crushing and squeezing |
| KR102437589B1 (en) * | 2021-11-19 | 2022-08-29 | 경기도 | Method of Manufacturing Perilla Oil with Reduced Specific Odor |
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