CN112481035A - Extraction method of fresh lotus essential oil - Google Patents
Extraction method of fresh lotus essential oil Download PDFInfo
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- CN112481035A CN112481035A CN202011295514.6A CN202011295514A CN112481035A CN 112481035 A CN112481035 A CN 112481035A CN 202011295514 A CN202011295514 A CN 202011295514A CN 112481035 A CN112481035 A CN 112481035A
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- 240000002853 Nelumbo nucifera Species 0.000 title claims abstract description 89
- 235000006508 Nelumbo nucifera Nutrition 0.000 title claims abstract description 89
- 235000006510 Nelumbo pentapetala Nutrition 0.000 title claims abstract description 89
- 239000000341 volatile oil Substances 0.000 title claims abstract description 51
- 238000000605 extraction Methods 0.000 title claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 230000007071 enzymatic hydrolysis Effects 0.000 claims abstract 5
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims abstract 5
- 108010059820 Polygalacturonase Proteins 0.000 claims description 7
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 7
- 108010002430 hemicellulase Proteins 0.000 claims description 7
- 229940059442 hemicellulase Drugs 0.000 claims description 7
- 108010059892 Cellulase Proteins 0.000 claims description 6
- 229940106157 cellulase Drugs 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 108090000790 Enzymes Proteins 0.000 claims description 2
- 102000004190 Enzymes Human genes 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229940088598 enzyme Drugs 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 102000011759 adducin Human genes 0.000 claims 1
- 108010076723 adducin Proteins 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 claims 1
- 239000001913 cellulose Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 239000003205 fragrance Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 11
- 239000003921 oil Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000005057 refrigeration Methods 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 241000628997 Flos Species 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 238000001256 steam distillation Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 210000000582 semen Anatomy 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000209477 Nymphaeaceae Species 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000209447 Nelumbo Species 0.000 description 1
- 235000005807 Nelumbo Nutrition 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 239000001525 mentha piperita l. herb oil Substances 0.000 description 1
- 235000019477 peppermint oil Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
本发明公开了一种新鲜荷花精油的提取方法，在荷花花瓣和花丝中喷洒酶解液后酶解，将酶解后的花瓣和花丝混合物粉碎后密封冷藏，加入乙醇后通入水蒸汽蒸馏，蒸馏3～4h后制得新鲜荷花精油。本发明以新鲜荷花为原料提取的荷花精油保留了新鲜荷花特有的淡雅花香，提高了荷花精油的质量和出油量，克服了荷花精油提取以干花为主、荷花干燥后香味损失较大、干花的精油香味成分较少以及质量较差的弊端。采用密封冷藏使荷花保存期可延长至3～5天，克服了新鲜荷花保存期短的弊端，有效提高了出油率，荷花精油提取率可提高20～30%，不仅得到质量上乘的新鲜荷花精油，同时保持了荷花特有的清香。
The invention discloses a method for extracting fresh lotus essential oil. The lotus flower petals and filaments are sprayed with an enzymatic hydrolysis solution and then enzymatically hydrolyzed, the enzymatically hydrolyzed petals and filaments mixture are pulverized, sealed and refrigerated, ethanol is added, and then steam is distilled for distillation. After 3 to 4 hours, fresh lotus essential oil was prepared. The lotus essential oil extracted from fresh lotus flower in the present invention retains the unique and elegant fragrance of fresh lotus flower, improves the quality and oil yield of lotus flower essential oil, and overcomes the problem that the lotus flower essential oil is mainly extracted from dried flowers, the fragrance loss of lotus flower is large after drying, and the dried flower The essential oil has the disadvantages of less fragrance components and poorer quality. The use of sealed and refrigerated storage can extend the shelf life of lotus flowers to 3 to 5 days, overcome the shortcoming of fresh lotus flowers, and effectively improve the oil yield. Essential oil, while maintaining the unique fragrance of lotus flowers.
Description
Background
The lotus belongs to a perennial aquatic perennial root herbaceous plant of Nymphaeaceae (Nymphaeaceae) and Nelumbo, and the flowering phase is 7-8 months per year. The lotus is originally produced in China and is one of the traditional Chinese medicines. According to the records of Ben Cao gang mu, lotus seeds, lotus coats, lotus houses, lotus stamens, lotus plumule, lotus leaves, lotus petioles, lotus nodes and the like of lotus can be used as the medicine. The lotus has ornamental value, and the lotus petals have the medicinal effects of promoting blood circulation, stopping bleeding, eliminating dampness, dispelling wind, clearing away the heart-fire, cooling blood, relieving fever, detoxifying and the like.
The volatile oil is also called essential oil, and is oily liquid with volatility capable of being distilled with water vapor, most of which has fragrance, such as rose essential oil, peppermint oil and the like. The volatile oil is insoluble in water and easily soluble in organic solvent.
The lotus has abundant planting resources in China, but the development and the utilization of the lotus are less, and the extraction of essential oil from fresh lotus as a raw material is rarely reported. The loss of fragrance of the lotus is large in the drying process, the fresh lotus contains rich fragrance substances, the fragrance is elegant, but the preservation of a large amount of fresh lotus in the actual production is difficult.
At present, the extraction method of lotus essential oil mostly adopts dried lotus, and is mostly used for experimental analysis.
CN103966023A discloses a method for extracting essence from lotus stamen, which comprises soaking lotus pollen and buds in organic solvent, and distilling to obtain the final product essence. The obtained flos Nelumbinis essence only contains fragrant substances dissolved in organic solvent, and not all flos Nelumbinis essential oil components.
CN104194934A discloses a preparation method of a lotus extract, which takes petroleum ether as an extracting agent and obtains the lotus extract by removing the petroleum ether through reduced pressure distillation. The lotus extract prepared by the method is difficult to apply in the fields of food, tobacco, medicine and the like because petroleum ether has certain toxicity and can be remained after reduced pressure distillation.
Disclosure of Invention
The invention provides a method for extracting fresh lotus essential oil, which is characterized in that a large amount of fragrance components in fresh lotus petals and filaments are extracted to obtain the fresh lotus essential oil with superior quality and keep the special faint scent of lotus.
In order to realize the purpose of the invention, the extraction method of the fresh lotus essential oil is characterized by comprising the following steps:
a. uniformly spraying 1-20% of enzymolysis liquid with mass concentration in fresh lotus petals and a filament raw material from which impurities such as receptacle, lotus seeds and the like are removed, and carrying out enzymolysis for 3-4 h at 30-38 ℃, wherein the enzymolysis liquid is an aqueous solution of cellulase, hemicellulase and pectinase, and the weight parts of the cellulase, hemicellulase and pectinase are as follows: 0.1-1: 0.05-0.5: 0.08-0.9, wherein the fresh lotus petals and the fresh lotus filaments are prepared from the raw materials and the enzymatic hydrolysate in parts by weight: 100-200: 1;
b. crushing the mixture of the petals and the filaments after enzymolysis to 20-40 meshes, then carrying out sealed refrigeration for 2-48 hours at 10-15 ℃ and 60-65% humidity, adding 95% ethanol, introducing 100-110 ℃ water vapor, distilling, and distilling for 3-4 hours to obtain fresh lotus essential oil, wherein the weight part ratio of the ethanol to the mixture of the petals and the filaments after enzymolysis is 0.1-1: 100, and the flow rate of the water vapor is 16 kg/h.
The invention achieves the technical progress that:
1. the lotus essential oil extracted by taking the fresh lotus as the raw material reserves the unique elegant fragrance of the fresh lotus, improves the quality and the oil output of the lotus essential oil, and overcomes the defects that the lotus essential oil is mainly extracted from the dried lotus, the fragrance loss is large after the lotus is dried, the fragrance component of the essential oil of the dried lotus is less, and the quality is poorer.
2. The invention adopts a sealed refrigeration method to prolong the retention period of the lotus to 3-5 days, and overcomes the defects of short retention period of the fresh lotus and short retention period of the fresh lotus in a high-temperature season.
3. The method adopts the methods of enzyme treatment, crushing, entrainer use and the like, effectively improves the oil yield of fresh flowers, can improve the extraction rate of the essential oil of the lotus by 20-30 percent compared with the existing steam distillation process, not only obtains the fresh essential oil of the lotus with superior quality by extracting a large amount of fragrant components in fresh lotus petals and filaments, but also keeps the unique faint scent of the lotus.
4. In order to overcome the defect that essential oil adheres to the inner wall of equipment, especially a condensation pipe, in the extraction process, the essential oil is collected for multiple times, the temperature of the condensation pipe is controlled by adjusting the amount of condensation water, the condensation water is closed before extraction is finished, and steam is continuously introduced to discharge the essential oil adhered to the condensation pipe and other pipelines, so that the extraction rate of the essential oil is effectively improved.
Drawings
FIG. 1 is a total ion flow diagram of the lotus essential oil of the present invention.
Detailed Description
Example 1:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 50g of cellulase, 25g of hemicellulase and 45g of pectinase, mixing, adding 1000ml of water, uniformly stirring, and uniformly spraying on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 35 ℃ for 3.5 hours;
d. crushing the petals and the filaments after enzymolysis to 40 meshes, performing sealed refrigeration at the temperature of 11 ℃ and the humidity of 60% for 15 hours, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 200mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at the steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the steam condensed water temperature at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after distillation for 3.5 hours, then continuing to introduce the steam for 0.5 hour, the fresh lotus essential oil attached in the discharge pipeline is collected for 5-6 times and then accumulated to obtain 12mL of fresh lotus essential oil.
Analyzing the fragrance components of the collected fresh lotus essential oil by adopting a GC/MS method, wherein the fragrance components are shown in the following table 1, and as can be seen from the fragrance components of the lotus essential oil, the lotus essential oil mainly contains compounds such as alkanes, alkenes, alcohols, enols, phenols, ethers, ketones, esters and the like, and the compounds such as alcohols, esters and olefins are abundant; the total ion flow diagram of the lotus essential oil is shown in figure 1.
Example 2:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 30g of cellulase, 50g of hemicellulase and 80g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 33 ℃ for 4 hours;
d. crushing the petals and the filaments after enzymolysis to 30 meshes, performing sealed refrigeration at 13 ℃ and 63% humidity for 20 hours, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 150mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at a steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the temperature of the steam condensed water at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after 3.5 hours of distillation, and then continuing to introduce the steam for 0.5 hours, the fresh lotus essential oil attached in the discharge pipeline is collected for 5-6 times and then accumulated to obtain 10mL of fresh lotus essential oil.
The flavor components of the collected fresh lotus essential oil were analyzed by GC/MS method, and the flavor components were not significantly different from those of example 1.
Example 3:
a. removing impurities such as receptacle and semen Nelumbinis from fresh flos Nelumbinis, and retaining petal and filament;
b. accurately weighing 60g of cellulase, 40g of hemicellulase and 50g of pectinase, mixing, adding 1000ml of water, stirring uniformly, and spraying uniformly on 100kg of the petal and filament materials;
c. carrying out enzymolysis on the petals and the filaments sprayed with the enzymolysis liquid at 38 ℃ for 3 hours;
d. crushing the petals and the filaments after enzymolysis to 20 meshes, performing sealed refrigeration for 8 hours at 15 ℃ and 65% humidity, then performing direct steam distillation on the petals and the filaments after the sealed refrigeration treatment by using a distillation still, arranging a perforated basket between a steam inlet and a steam outlet, placing the petals and the filaments after the refrigeration treatment in the perforated basket, adding 550mL of 95% ethanol entrainer, adding the entrainer ethanol to promote evaporation of volatile components in the distillation process, then introducing 100-110 ℃ steam, performing distillation at a steam flow rate of 16kg/h, adjusting the amount of condensed water in the distillation extraction process to keep the temperature of the steam condensed water at about 70 ℃, when the amount of fresh lotus essential oil in an oil-water separator is more than 1mL, collecting fresh lotus essential oil by using a separating funnel, closing the condensed water after 3.5 hours of distillation, and then continuing to introduce the steam for 0.5 hours, the fresh lotus essential oil attached in the discharge pipeline is collected for 5-6 times and then accumulated to obtain 9mL of fresh lotus essential oil.
The flavor components of the collected fresh lotus essential oil were analyzed by GC/MS method, and the flavor components were not significantly different from those of example 1.
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| CN202011295514.6A CN112481035A (en) | 2020-11-18 | 2020-11-18 | Extraction method of fresh lotus essential oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232670A (en) * | 2022-06-15 | 2022-10-25 | 河北中烟工业有限责任公司 | Lotus essence and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090076536A (en) * | 2008-01-09 | 2009-07-13 | 동국대학교 산학협력단 | Lotus extract having skin treatment effect and preparation method thereof |
| CN104194934A (en) * | 2014-08-29 | 2014-12-10 | 杨祝华 | Preparation method of lotus extractum |
| CN108315098A (en) * | 2018-03-14 | 2018-07-24 | 海南大学 | A kind of Nymphaea caerulea method of extraction of essential oil and its application |
| CN109628221A (en) * | 2018-11-29 | 2019-04-16 | 广州柚子舍生物科技有限公司 | The extracting method of shaddock flower essential oil |
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2020
- 2020-11-18 CN CN202011295514.6A patent/CN112481035A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| KR20090076536A (en) * | 2008-01-09 | 2009-07-13 | 동국대학교 산학협력단 | Lotus extract having skin treatment effect and preparation method thereof |
| CN104194934A (en) * | 2014-08-29 | 2014-12-10 | 杨祝华 | Preparation method of lotus extractum |
| CN108315098A (en) * | 2018-03-14 | 2018-07-24 | 海南大学 | A kind of Nymphaea caerulea method of extraction of essential oil and its application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115232670A (en) * | 2022-06-15 | 2022-10-25 | 河北中烟工业有限责任公司 | Lotus essence and preparation method thereof |
| CN115232670B (en) * | 2022-06-15 | 2023-11-28 | 河北中烟工业有限责任公司 | Lotus essence and preparation method thereof |
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