CN115444135A - Shaddock peel extraction process and shaddock peel extract - Google Patents
Shaddock peel extraction process and shaddock peel extract Download PDFInfo
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- CN115444135A CN115444135A CN202210637068.5A CN202210637068A CN115444135A CN 115444135 A CN115444135 A CN 115444135A CN 202210637068 A CN202210637068 A CN 202210637068A CN 115444135 A CN115444135 A CN 115444135A
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- peel
- shaddock
- liquid
- pomelo peel
- pomelo
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- 244000276331 Citrus maxima Species 0.000 title claims abstract description 197
- 235000001759 Citrus maxima Nutrition 0.000 title claims abstract description 86
- 239000000284 extract Substances 0.000 title claims abstract description 76
- 238000000605 extraction Methods 0.000 title claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 73
- 238000004821 distillation Methods 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 81
- 239000002994 raw material Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 16
- 240000000560 Citrus x paradisi Species 0.000 claims description 13
- -1 polyethylene Polymers 0.000 claims description 13
- 239000004698 Polyethylene Substances 0.000 claims description 12
- 229920000573 polyethylene Polymers 0.000 claims description 12
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 235000012907 honey Nutrition 0.000 claims description 2
- 241000907663 Siproeta stelenes Species 0.000 claims 1
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 abstract description 16
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
- 238000012545 processing Methods 0.000 abstract description 10
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 abstract description 8
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 abstract description 8
- 235000001510 limonene Nutrition 0.000 abstract description 8
- 229940087305 limonene Drugs 0.000 abstract description 8
- 229930007744 linalool Natural products 0.000 abstract description 8
- 150000004676 glycans Chemical class 0.000 abstract description 7
- 229920001282 polysaccharide Polymers 0.000 abstract description 7
- 239000005017 polysaccharide Substances 0.000 abstract description 7
- 239000000796 flavoring agent Substances 0.000 abstract description 6
- 235000019634 flavors Nutrition 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- BAVONGHXFVOKBV-UHFFFAOYSA-N Carveol Chemical compound CC(=C)C1CC=C(C)C(O)C1 BAVONGHXFVOKBV-UHFFFAOYSA-N 0.000 description 8
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- BAVONGHXFVOKBV-ZJUUUORDSA-N (-)-trans-carveol Natural products CC(=C)[C@@H]1CC=C(C)[C@@H](O)C1 BAVONGHXFVOKBV-ZJUUUORDSA-N 0.000 description 4
- WECGLUPZRHILCT-GSNKCQISSA-N 1-linoleoyl-sn-glycerol Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OC[C@@H](O)CO WECGLUPZRHILCT-GSNKCQISSA-N 0.000 description 4
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 4
- 235000021355 Stearic acid Nutrition 0.000 description 4
- 229930007646 carveol Natural products 0.000 description 4
- YCOZIPAWZNQLMR-UHFFFAOYSA-N heptane - octane Natural products CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000008117 stearic acid Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 244000241257 Cucumis melo Species 0.000 description 2
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 2
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- NDVASEGYNIMXJL-UHFFFAOYSA-N sabinene Chemical compound C=C1CCC2(C(C)C)C1C2 NDVASEGYNIMXJL-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GRWFGVWFFZKLTI-UHFFFAOYSA-N α-pinene Chemical compound CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 2
- NDVASEGYNIMXJL-NXEZZACHSA-N (+)-sabinene Natural products C=C1CC[C@@]2(C(C)C)[C@@H]1C2 NDVASEGYNIMXJL-NXEZZACHSA-N 0.000 description 1
- GAIBLDCXCZKKJE-QRYCCKSOSA-N (-)-Germacrene D Natural products C(C)(C)[C@H]1/C=C/C(=C)CC/C=C(/C)\CC1 GAIBLDCXCZKKJE-QRYCCKSOSA-N 0.000 description 1
- GRWFGVWFFZKLTI-IUCAKERBSA-N 1S,5S-(-)-alpha-Pinene Natural products CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 description 1
- 244000183685 Citrus aurantium Species 0.000 description 1
- 235000007716 Citrus aurantium Nutrition 0.000 description 1
- 235000000228 Citrus myrtifolia Nutrition 0.000 description 1
- 235000016646 Citrus taiwanica Nutrition 0.000 description 1
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 1
- 239000005792 Geraniol Substances 0.000 description 1
- GAIBLDCXCZKKJE-YZJXYJLZSA-N Germacren D Chemical compound CC(C)C/1CC\C(C)=C\CCC(=C)\C=C\1 GAIBLDCXCZKKJE-YZJXYJLZSA-N 0.000 description 1
- GLZPCOQZEFWAFX-JXMROGBWSA-N Nerol Natural products CC(C)=CCC\C(C)=C\CO GLZPCOQZEFWAFX-JXMROGBWSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 description 1
- KQAZVFVOEIRWHN-UHFFFAOYSA-N alpha-thujene Natural products CC1=CCC2(C(C)C)C1C2 KQAZVFVOEIRWHN-UHFFFAOYSA-N 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 229940043350 citral Drugs 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 1
- HIGQPQRQIQDZMP-UHFFFAOYSA-N geranil acetate Natural products CC(C)=CCCC(C)=CCOC(C)=O HIGQPQRQIQDZMP-UHFFFAOYSA-N 0.000 description 1
- 229940113087 geraniol Drugs 0.000 description 1
- HIGQPQRQIQDZMP-DHZHZOJOSA-N geranyl acetate Chemical compound CC(C)=CCC\C(C)=C\COC(C)=O HIGQPQRQIQDZMP-DHZHZOJOSA-N 0.000 description 1
- OJIGFVZZEVQUNV-UHFFFAOYSA-N germacrene D Natural products CC(C)C1CCC=C(/C)CCC(=C)C=C1 OJIGFVZZEVQUNV-UHFFFAOYSA-N 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- GAIBLDCXCZKKJE-UHFFFAOYSA-N isogermacrene D Natural products CC(C)C1CCC(C)=CCCC(=C)C=C1 GAIBLDCXCZKKJE-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229930006696 sabinene Natural products 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
- A23L5/276—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- 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
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Nutrition Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Botany (AREA)
- Mycology (AREA)
- Seasonings (AREA)
Abstract
The invention relates to the field of A23L33/105, in particular to a shaddock peel extraction process and a shaddock peel extract. The invention provides a pomelo peel extraction process and a pomelo peel extract, which have the advantages of simple process and high extraction rate, fully utilize the pomelo peel resources discarded during pomelo processing, ensure the extraction rate, quality and safety of the pomelo peel extract on the premise of not influencing the aroma and flavor of the pomelo peel extract and are beneficial to subsequent large-scale comprehensive utilization on the basis of the application requirements and application prospects of rich pomelo peel polysaccharide, limonene, linalool and other components in the pomelo peel in the fields of food, essence and daily chemicals by designing the pomelo peel extraction process at least comprising the steps of soaking, cleaning, crushing, squeezing, vibrating, standing for layering, liquid-liquid separation, upper-layer pressure distillation and lower-layer distillation.
Description
Technical Field
The invention relates to the field of A23L33/105, in particular to a pomelo peel extraction process and a pomelo peel extract.
Background
Pomelo is an important economic crop, and is planted in large area in southern areas of China, but the pomelo peel with the fresh weight of 20-30% cannot be utilized in the production process of the pomelo, and the pomelo peel contains various components, mainly including terpenes (limonene, germacrene D, alpha-pinene and sabinene), alcohols (linalool, nerol, geraniol and the like), esters (geranyl acetate) and aldehydes (citral and citrus aurantium aldehyde), and also contains a certain amount of phenols, benzenes, oxides, alkanes, ketones and other components, so that the waste of rich resources in the pomelo peel is caused.
Chinese patent CN104666226B discloses a floral water containing pericarpium Citri Grandis extract and its preparation method, which adopts petroleum ether solvent extraction method to prepare pericarpium Citri Grandis extract, but the pericarpium Citri Grandis extract product obtained by the method has solvent residue, which affects safety and quality of pericarpium Citri Grandis extract, and is not beneficial to retaining fragrance and flavor of pericarpium Citri Grandis extract; chinese patent CN112841649A discloses a pomelo peel extract and a preparation method and application thereof, wherein the pomelo peel extract is prepared by shearing and emulsifying raw materials such as pomelo peel materials, water and inorganic salt, carrying out solid-liquid separation, and carrying out subsequent treatment, although organic solvent residue is reduced to a certain degree, the treatment process is complex in process operation, large in production equipment investment and not beneficial to large-scale industrial production.
Therefore, based on the application requirements and application prospects of rich pomelo peel polysaccharide, limonene, linalool and other components in the pomelo peel in the fields of food, essence and daily chemicals, a pomelo peel extraction process and a pomelo peel extract with simple process and high extraction rate are provided, the pomelo peel resource discarded in pomelo processing is fully utilized, the extraction rate, quality and safety of the pomelo peel extract are ensured on the premise of not influencing the aroma and flavor of the pomelo peel extract, and the follow-up large-scale comprehensive utilization is facilitated.
Disclosure of Invention
In order to solve the problems, the invention provides a shaddock ped extraction process which at least comprises the steps of soaking and cleaning, crushing, squeezing, vibrating, standing and layering, liquid-liquid separation, upper layer pressure distillation and lower layer distillation.
As a preferable technical scheme, the pomelo peel extraction process at least comprises the following steps:
s1, performing peel and pulp separation on a shaddock peel raw material, soaking the shaddock peel raw material into a saline solution for 5-10min, and then cleaning the shaddock peel raw material with clear water;
s2, cutting the cleaned shaddock peel into shaddock peel pieces of (2-3) cm, and crushing the shaddock peel pieces in a crusher;
s3, placing the crushed shaddock peel material into a squeezer for squeezing, collecting effluent liquid, and stopping squeezing after no obvious liquid flows out;
s4, filling the outflow liquid collected in the step S3 into a bottle made of a specific material, and adding dichloromethane for vibration;
s5, standing the vibrated liquid for 12-13h, and separating the upper-layer liquid from the lower-layer liquid;
s6, distilling the lower-layer liquid in a water bath until no liquid drips out from a condensation port to obtain a pomelo peel extract A;
s7, distilling the upper layer liquid under pressure until no liquid overflows to obtain the pomelo peel extract B.
As a preferred technical scheme, in the step S1, the pomelo peel raw material is from pomelo peel which is a by-product of pomelo processing, and the by-product of pomelo processing is effectively utilized, so that the environment pollution caused by the waste pomelo peel and the waste of pomelo peel resources are avoided; preferably, the shaddock peel is one of a grapefruit peel, a Majia shaddock peel, a four-season shaddock peel, a shatian shaddock peel, a white shaddock peel and a honey shaddock peel;
as a preferable technical scheme, in the step S1, the mass fraction of sodium chloride in the saline solution is 2-5%, because the pomelo peel raw material is from a by-product pomelo peel produced from pomelo, the collected pomelo peel raw material is separated from melon pulp and then soaked in the saline solution with the mass fraction of sodium chloride of 2-5% for 5-10min and then washed with clear water, so that impurities and bacteria on the surface of the pomelo peel raw material are removed, the impurities carried in the raw material are prevented from affecting the subsequent extraction process, and the quality and safety of the extract are ensured.
As a preferable technical scheme, in the step S2, the rotation speed of the crusher is 1000-2000 rpm, and the crushing time is 1-2min; the inventor finds that the crushing degree of the pomelo peel directly influences the extraction rate of the pomelo peel extract in the research process, and controls the crushing degree of the pomelo peel raw material by controlling the rotating speed of the crusher to be 1000-2000 r/min and the crushing time to be 1-2min, so that the contact area between the pomelo peel raw material and dichloromethane is ensured, and the extraction efficiency and the extraction rate of the pomelo peel extract are further ensured.
As a preferable technical scheme, the bottle made of a specific material in the step S4 is a polyethylene bottle, so that the polyethylene bottle has high stability to dichloromethane, the adhesion of the effluent liquid to the bottle wall is reduced, and the reduction of the extraction rate of the pomelo peel extract caused by the adhesion of active ingredients in the effluent liquid to the bottle wall is avoided;
as a preferable technical solution, the mass ratio of the effluent liquid to the dichloromethane in the step S4 is (1-2): (1.5-5);
as a preferred technical solution, the vibration in step S4 is specifically: and (3) placing the polyethylene bottle filled with the effluent liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 15-25 ℃, and vibrating for 1.5-3h by using the vibrating screen. In the actual extraction exploration process, in order to simultaneously meet the requirements of realizing the economy, safety and high product quality of large-scale industrial production, the inventor controls the mass ratio of the effluent liquid to the dichloromethane to be (1-2): (1.5-5), on the premise of ensuring the extraction effect, the raw material cost and the post-treatment cost caused by excessive use of dichloromethane are reduced, and the economy is improved; in addition, the inventor finds that the temperature and the vibration time in the vibration process stipulate the uniform contact and exchange degree between the outflow liquid and dichloromethane, and further influence the extraction rate and the product quality of the pomelo peel extract, and the inventor conducts a large amount of creative tests to obtain the pomelo peel extract, and the method controls the temperature to be 15-25 ℃, adopts a vibration screen to vibrate for 1.5-3h, so that the vibration contact and exchange between the outflow liquid and the dichloromethane are complete, and further improves the extraction rate of the pomelo peel extract and ensures the product quality and safety on the premise of not influencing the aroma and the flavor of the pomelo peel extract.
As a preferred technical scheme, the temperature of the water bath distillation in the step S6 is 60-70 ℃; preferably, the pomelo peel extract A at least comprises limonene, linalool, carveol, linoleic acid glyceride, stearic acid glyceride and n-tetradecane;
as a preferable technical scheme, the temperature of the pressure distillation in the step S7 is 78-82 ℃, and the pressure is 0.1-0.2atm; preferably, the pomelo peel extract B at least comprises pomelo peel polysaccharide;
the invention also provides a pomelo peel extract obtained by adopting a pomelo peel extraction process, wherein the pomelo peel extract comprises a pomelo peel extract A and a pomelo peel extract B.
Has the advantages that:
1. based on the application requirements and application prospects of rich pomelo peel polysaccharide, limonene, linalool and other components in the pomelo peel in the fields of food, essence and daily chemicals, the invention provides a pomelo peel extraction process and a pomelo peel extract with simple process and high extraction rate, which fully utilize the pomelo peel resources discarded in pomelo processing, ensure the extraction rate, quality and safety of the pomelo peel extract on the premise of not influencing the aroma and flavor of the pomelo peel extract, and are beneficial to subsequent large-scale comprehensive utilization.
2. The shaddock peel raw materials in this application come from shaddock processing accessory substance shaddock peel, carry out effective utilization with shaddock processing accessory substance, avoid abandonment shaddock peel polluted environment and the waste of shaddock peel resource, carry out the shaddock peel raw materials that will collect and soak to soak 5-10min of the mass fraction of sodium chloride for soaking in 2-5% salt water after the melon pulp separation, wash with the clear water, detach the impurity and the bacterium on shaddock peel raw materials surface, avoid the impurity that carries in the raw materials to influence follow-up extraction technology, guarantee extract quality and safety.
3. The invention controls the crushing degree of the pomelo peel raw material by controlling the rotating speed of the crusher to be 1000-2000 r/min and the crushing time to be 1-2min, thereby ensuring the contact area between the pomelo peel raw material and dichloromethane and further ensuring the extraction efficiency and the extraction rate of the pomelo peel extract.
4. The invention controls the mass ratio of the effluent liquid to the dichloromethane to be (1-2): (1.5-5), on the premise of ensuring the extraction effect, the raw material cost and the post-treatment cost caused by excessive use of dichloromethane are reduced, and the economy is improved; and then, by controlling the temperature to be 15-25 ℃, vibrating for 1.5-3h by adopting a vibrating screen, the vibration contact exchange between the outflow liquid and dichloromethane is complete, the extraction rate of the pomelo peel extract is improved, and the product quality and safety are ensured on the premise of not influencing the aroma and flavor of the pomelo peel extract.
Detailed Description
Example 1
In one aspect, embodiment 1 of the invention provides a pomelo peel extraction process, which comprises the following steps:
s1, separating peel and pulp of a shaddock peel raw material, soaking the shaddock peel raw material into a salt water solution for 10min, and then cleaning the shaddock peel raw material with clear water;
s2, cutting the cleaned shaddock peel into 2cm-2cm shaddock peel sheets, and crushing the shaddock peel sheets in a crusher;
s3, placing the crushed shaddock peel material into a squeezer for squeezing, collecting effluent liquid, and stopping squeezing after no obvious liquid flows out;
s4, filling the outflow liquid collected in the step S3 into a bottle made of a specific material, and adding dichloromethane for vibration;
s5, standing the vibrated liquid for 12 hours, and separating the upper-layer liquid from the lower-layer liquid;
s6, distilling the lower-layer liquid in a water bath until no liquid drips out from a condensation port to obtain a pomelo peel extract A;
s7, distilling the upper layer liquid under pressure until no liquid overflows to obtain the pomelo peel extract B.
In the step S1, the shaddock peel raw material is prepared from a shaddock processing by-product shaddock peel, and the shaddock peel is a grapefruit peel;
in the step S1, the mass fraction of sodium chloride in the saline solution is 3%.
In the step S2, the rotating speed of the pulverizer is 1500 revolutions per minute, and the pulverizing time is 1.5min.
S4, the bottle made of the specific material is a polyethylene bottle;
the mass ratio of the effluent liquid to the dichloromethane in the step S4 is 1.5:3;
the step S4 of vibrating specifically includes: and (3) placing the polyethylene bottle filled with the effluent liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 20 ℃, and vibrating for 2 hours by using the vibrating screen.
The temperature of water bath distillation in the step S6 is 65 ℃; the pomelo peel extract A comprises limonene, linalool, carveol, linoleic acid glyceride, stearic acid glyceride and n-tetradecane;
the temperature of the pressure distillation in the step S7 is 80 ℃, and the pressure is 0.15atm; the pomelo peel extract B is pomelo peel polysaccharide;
in another aspect, embodiment 1 of the present invention provides a pomelo peel extract obtained by using a pomelo peel extraction process, wherein the pomelo peel extract comprises a pomelo peel extract a and a pomelo peel extract B.
Example 2
In one aspect, embodiment 2 of the invention provides a pomelo peel extraction process, which comprises the following steps:
s1, separating peel and pulp of a shaddock peel raw material, soaking the shaddock peel raw material into a salt water solution for 10min, and then cleaning the shaddock peel raw material with clear water;
s2, cutting the cleaned shaddock peel into 2cm-2 cm shaddock peel slices, and crushing the shaddock peel slices in a crusher;
s3, placing the crushed shaddock peel material in a squeezer for squeezing, collecting effluent liquid, and stopping squeezing after no obvious liquid flows out;
s4, filling the outflow liquid collected in the step S3 into a bottle made of a specific material, and adding dichloromethane for vibration;
s5, standing the vibrated liquid for 12 hours, and separating the upper-layer liquid from the lower-layer liquid;
s6, distilling the lower-layer liquid in a water bath until no liquid drips out from a condensation port to obtain a pomelo peel extract A;
s7, distilling the upper layer liquid under pressure until no liquid overflows to obtain the pomelo peel extract B.
In the step S1, the shaddock peel raw material is obtained from a shaddock processing by-product shaddock peel, and the shaddock peel is a shaddock peel;
in the step S1, the mass fraction of sodium chloride in the saline solution is 3%.
In the step S2, the rotating speed of the pulverizer is 1800 revolutions per minute, and the pulverizing time is 1.2min.
S4, the bottle made of the specific material is a polyethylene bottle;
the mass ratio of the effluent liquid to the dichloromethane in the step S4 is 1.5:2.8;
the step S4 of vibrating specifically includes: and (3) placing the polyethylene bottle filled with the outflow liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 25 ℃, and vibrating for 1.8h by using the vibrating screen.
The temperature of water bath distillation in the step S6 is 70 ℃; the pomelo peel extract A comprises limonene, linalool, carveol, linoleic acid glyceride, stearic acid glyceride and n-tetradecane;
the temperature of the pressure distillation in the step S7 is 82 ℃, and the pressure is 0.2atm; the pomelo peel extract B is pomelo peel polysaccharide;
in another aspect, embodiment 2 of the present invention provides a pomelo peel extract obtained by using a pomelo peel extraction process, wherein the pomelo peel extract comprises a pomelo peel extract a and a pomelo peel extract B.
Example 3
In one aspect, the embodiment 3 of the invention provides a shaddock peel extraction process, which comprises the following steps:
s1, separating peel and pulp of a shaddock peel raw material, soaking the shaddock peel raw material into a salt water solution for 8min, and then cleaning the shaddock peel raw material with clear water;
s2, cutting the cleaned shaddock peel into 2cm-2 cm shaddock peel slices, and crushing the shaddock peel slices in a crusher;
s3, placing the crushed shaddock peel material in a squeezer for squeezing, collecting effluent liquid, and stopping squeezing after no obvious liquid flows out;
s4, filling the outflow liquid collected in the step S3 into a bottle made of a specific material, and adding dichloromethane for vibration;
s5, standing the vibrated liquid for 12 hours, and separating the upper-layer liquid from the lower-layer liquid;
s6, distilling the lower-layer liquid in a water bath until no liquid drips out from a condensation port to obtain a pomelo peel extract A;
s7, distilling the upper layer liquid under pressure until no liquid overflows to obtain the pomelo peel extract B.
In the step S1, the shaddock peel raw material is prepared from a shaddock processing by-product shaddock peel, and the shaddock peel is a citrus grandis peel;
in the step S1, the mass fraction of sodium chloride in the saline solution is 4%.
In the step S2, the rotating speed of the pulverizer is 1200 revolutions per minute, and the pulverizing time is 2min.
S4, the bottle made of the specific material is a polyethylene bottle;
the mass ratio of the effluent liquid to the dichloromethane in the step S4 is 1.5:3.2;
the step S4 of vibrating specifically includes: and (3) placing the polyethylene bottle filled with the outflow liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 18 ℃, and vibrating for 2.5 hours by using the vibrating screen.
The temperature of the water bath distillation in the step S6 is 62 ℃; the pomelo peel extract A comprises limonene, linalool, carveol, linoleic acid glyceride, stearic acid glyceride and n-tetradecane;
the temperature of the pressure distillation in the step S7 is 78 ℃, and the pressure is 0.1atm; the pomelo peel extract B is pomelo peel polysaccharide;
in another aspect, embodiment 3 of the present invention provides a pomelo peel extract obtained by using a pomelo peel extraction process, wherein the pomelo peel extract comprises a pomelo peel extract a and a pomelo peel extract B.
Comparative example 1
The comparative example 1 of the invention provides a shaddock ped extraction process, and the specific implementation mode of the process is the same as that of the example 1, except that the rotation speed of a crusher in the step S2 is 3000 r/min, and the crushing time is 30S.
Comparative example 2
The comparative example 2 of the invention provides a shaddock ped extraction process, which is the same as the embodiment 1 in the specific implementation manner, and is different from the step 1 in that the mass ratio of the effluent liquid to dichloromethane in the step S4 is 1.5:2.
comparative example 3
A comparative example 3 of the present invention provides a shaddock ped extraction process, which is the same as example 1 in specific implementation manner, and the difference is that the vibration in the step S4 specifically includes: and (3) placing the polyethylene bottle filled with the effluent liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 40 ℃, and vibrating for 1 hour by using the vibrating screen.
Performance test method
The extraction rate of the pomelo peel extract obtained using the pomelo peel extraction process provided in examples and comparative examples was calculated by the formula (extraction rate = pomelo peel extract weight/pomelo peel raw material weight × 100%, where pomelo peel extract weight is the sum of pomelo peel extract a weight and pomelo peel extract B weight), and the results are shown in table 1.
Referring to table 1, table 1 shows performance test data of the grapefruit peel extracts prepared by the specific processes of examples 1 to 3 and comparative examples 1 to 3.
| Test item | Extraction ratio (wt%) |
| Example 1 | 3.2 |
| Example 2 | 3.15 |
| Example 3 | 3.0 |
| Comparative example 1 | 2.83 |
| Comparative example 2 | 2.75 |
| Comparative example 3 | 2.66 |
Claims (10)
1. A pomelo peel extraction process is characterized by at least comprising the steps of soaking, cleaning, crushing, squeezing, vibrating, standing, layering, liquid-liquid separation, upper-layer pressure distillation and lower-layer distillation.
2. The shaddock ped extraction process as recited in claim 1, comprising at least the steps of:
s1, performing peel and pulp separation on a shaddock peel raw material, soaking the shaddock peel raw material into a saline solution for 5-10min, and then cleaning the shaddock peel raw material with clear water;
s2, cutting the cleaned shaddock peel into shaddock peel pieces of (2-3) cm, and crushing the shaddock peel pieces in a crusher;
s3, placing the crushed shaddock peel material into a squeezer for squeezing, collecting effluent liquid, and stopping squeezing after no obvious liquid flows out;
s4, filling the outflow liquid collected in the step S3 into a bottle made of a specific material, and adding dichloromethane for vibration;
s5, standing the vibrated liquid for 12-13h, and separating the upper-layer liquid from the lower-layer liquid;
s6, distilling the lower-layer liquid in a water bath until no liquid drips out from a condensation port to obtain a pomelo peel extract A;
s7, distilling the upper layer liquid under pressure until no liquid overflows to obtain the pomelo peel extract B.
3. The shaddock peel extraction process according to claim 2, wherein the shaddock peel is one of a grapefruit peel, a malachite peel, a four-season shaddock peel, a shatian shaddock peel, a white shaddock peel and a honey shaddock peel.
4. The shaddock ped extraction process according to claim 2, wherein the mass fraction of sodium chloride in the saline solution in step S1 is 2-5%.
5. The shaddock ped extraction process according to claim 2, wherein the rotation speed of the crusher in the step S2 is 1000-2000 rpm, and the crushing time is 1-2min.
6. The shaddock ped extraction process of claim 2, wherein the bottles made of the specific material in step S4 are polyethylene bottles.
7. The shaddock ped extraction process as recited in claim 2, wherein the mass ratio of the effluent liquid to the dichloromethane in the step S4 is (1-2): (1.5-5).
8. The shaddock ped extraction process according to claim 1, wherein the vibration in the step S4 is specifically: and (3) placing the polyethylene bottle filled with the outflow liquid and the dichloromethane on a vibrating screen for fixing, controlling the temperature to be 15-25 ℃, and vibrating for 1.5-3h by using the vibrating screen.
9. The extraction process of pomelo peel as claimed in claim 2, wherein the temperature of the water bath distillation in the step S6 is 60-70 ℃.
10. A pomelo peel extract prepared by a pomelo peel extraction process according to any one of claims 1 to 9, wherein the pomelo peel extract comprises a pomelo peel extract a and a pomelo peel extract B.
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