CN115806859A - Method for extracting pepper essential oil and pepper essential oil prepared by same - Google Patents
Method for extracting pepper essential oil and pepper essential oil prepared by same Download PDFInfo
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- 235000008184 Piper nigrum Nutrition 0.000 title claims abstract description 247
- 235000002566 Capsicum Nutrition 0.000 title claims abstract description 246
- 239000006002 Pepper Substances 0.000 title claims abstract description 246
- 235000016761 Piper aduncum Nutrition 0.000 title claims abstract description 246
- 235000017804 Piper guineense Nutrition 0.000 title claims abstract description 246
- 239000000341 volatile oil Substances 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 65
- 241000722363 Piper Species 0.000 title claims abstract 29
- 238000000605 extraction Methods 0.000 claims abstract description 80
- 239000002994 raw material Substances 0.000 claims abstract description 78
- 239000003921 oil Substances 0.000 claims abstract description 60
- 238000000199 molecular distillation Methods 0.000 claims abstract description 41
- 239000001273 butane Substances 0.000 claims description 6
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- MXXWOMGUGJBKIW-YPCIICBESA-N piperine Chemical compound C=1C=C2OCOC2=CC=1/C=C/C=C/C(=O)N1CCCCC1 MXXWOMGUGJBKIW-YPCIICBESA-N 0.000 abstract description 68
- 229940075559 piperine Drugs 0.000 abstract description 68
- WVWHRXVVAYXKDE-UHFFFAOYSA-N piperine Natural products O=C(C=CC=Cc1ccc2OCOc2c1)C3CCCCN3 WVWHRXVVAYXKDE-UHFFFAOYSA-N 0.000 abstract description 68
- 235000019100 piperine Nutrition 0.000 abstract description 68
- 239000000447 pesticide residue Substances 0.000 abstract description 25
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229930014626 natural product Natural products 0.000 abstract description 2
- 244000203593 Piper nigrum Species 0.000 description 219
- 239000000110 cooling liquid Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 14
- 239000012071 phase Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000000047 product Substances 0.000 description 10
- 238000001704 evaporation Methods 0.000 description 8
- 239000005807 Metalaxyl Substances 0.000 description 7
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical group CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- ZQEIXNIJLIKNTD-UHFFFAOYSA-N methyl N-(2,6-dimethylphenyl)-N-(methoxyacetyl)alaninate Chemical compound COCC(=O)N(C(C)C(=O)OC)C1=C(C)C=CC=C1C ZQEIXNIJLIKNTD-UHFFFAOYSA-N 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000000194 supercritical-fluid extraction Methods 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000008601 oleoresin Substances 0.000 description 3
- 239000005944 Chlorpyrifos Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 235000013614 black pepper Nutrition 0.000 description 1
- 239000007891 compressed tablet Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000000554 physical therapy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 235000013599 spices Nutrition 0.000 description 1
- 235000019654 spicy taste Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to the technical field of natural product extraction, and particularly relates to a method for extracting pepper essential oil and the pepper essential oil prepared by the method. The invention provides a method for extracting pepper essential oil, which comprises the following steps: performing subcritical extraction on the pepper raw material to obtain pepper oil, performing molecular distillation on the pepper oil, and collecting a light phase. The method can ensure that the piperine is less extracted and the loss of the piperine is reduced while ensuring the higher extraction yield of the pepper essential oil, thereby obviously improving the content of the piperine in the pepper raw material after the extraction of the essential oil; the extraction method can also effectively remove pesticide residues in the pepper raw material, and ensure low pesticide residues in the pepper raw material after the pepper essential oil is extracted. In addition, the method has the characteristics of convenient operation and industrial production.
Description
Technical Field
The invention relates to the technical field of natural product extraction, and particularly relates to a method for extracting pepper essential oil and the pepper essential oil prepared by the method.
Background
Pepper, especially black pepper, contains abundant essential oil and flavor components such as piperine, and is a spice widely used at present. The pepper essential oil is a component providing characteristic aroma in pepper and has pepper characteristic aroma, the piperine is a component providing spicy taste in pepper, and the pepper essential oil and the piperine are widely applied to a plurality of fields of food, perfume, physical therapy and the like.
The traditional production method of pepper essential oil is steam distillation or supercritical extraction. The steam distillation method comprises the steps of crushing the pepper raw material, introducing high-temperature steam, carrying the essential oil out by the steam, condensing to form liquid, and separating from water to obtain the pepper essential oil.
The supercritical extraction method comprises the steps of crushing the pepper raw material, extracting with supercritical carbon dioxide, evaporating the extract to obtain supercritical pepper oil, wherein the pepper oil obtained by the method contains about 10-15% of piperine, so that the content of the piperine in the extracted pepper raw material is greatly reduced, and the product quality of the subsequently extracted pepper oleoresin is influenced.
Patent application CN107927696A uses supercritical carbon dioxide to extract crushed pepper raw material, after stirring, standing and dividing into 3 layers, wherein the upper layer yellowish transparent clear liquid and the middle layer yellow semi-solid product are filtered to obtain filtrate, the filtrate is mixed to obtain pepper essential oil, and the yellow solid obtained by suction filtration is pepper oleoresin, so that piperine is extracted simultaneously in the extraction process of the above method, which results in the quality reduction of pepper raw material after extraction of essential oil.
In view of the above, there is a need to develop an extraction method that can reduce the loss of piperine and ensure a high piperine content in the pepper raw material after extraction of essential oil.
Disclosure of Invention
The invention aims to provide a method for extracting pepper essential oil and the pepper essential oil prepared by the method.
The invention aims to reduce the piperine loss in the extraction process of the pepper essential oil and reduce the content of the piperine extracted in the extraction process of the pepper essential oil, and develops a method for extracting the pepper essential oil. The main effective components in the pepper raw material are pepper essential oil and piperine, the thermal stability of the piperine is poor, more loss can occur at higher temperature, the product quality of the pepper resin after the extraction of the essential oil is reduced, and the subsequent processed product does not meet the standard. In addition, the pepper raw material generally contains high pesticide residue, so the pesticide residue in the pepper raw material also needs to be removed as much as possible in the extraction process of pepper essential oil. In the research and development process, the invention finds that the existing common pepper essential oil extraction method is difficult to simultaneously ensure higher essential oil yield and lower piperine loss, and high piperine retention rate and low pesticide residue in pepper raw materials after essential oil extraction. The extraction method of the invention is obtained by carrying out a plurality of attempts on the extraction method of the pepper essential oil.
Specifically, the invention provides the following technical scheme:
the invention provides a method for extracting pepper essential oil, which comprises the following steps: performing subcritical extraction on pepper raw materials to obtain pepper oil, performing molecular distillation on the pepper oil, and collecting a light phase.
Compared with other extraction methods, the method adopting subcritical extraction combined with molecular distillation is more beneficial to reducing the loss of piperine and keeping the piperine in the raw materials left after the extraction of essential oil, and is also beneficial to removing pesticide residues in the pepper raw materials.
In addition, the present invention has also found that, unexpectedly, the processing temperature and moisture content of the pepper raw material before the subcritical extraction directly affect the product quality of the pepper oil obtained by the subcritical extraction, and the product quality of the pepper oil directly affects the extraction effect of the molecular distillation. The processing method of freezing the pepper raw material and then tabletting and controlling the moisture content of the pressed pepper raw material is adopted, so that the loss of piperine can be reduced while the yield of the pepper essential oil is obviously improved, the content of the piperine in the pepper raw material after the extraction of the essential oil is improved, pesticide components can be promoted to enter the pepper oil in the subcritical extraction process, and the low pesticide residue in the residual raw material after the extraction of the essential oil is better ensured.
Specifically, before the subcritical extraction, the pepper raw material is frozen and then tabletted, and the water content of the tabletted pepper raw material is 15-20%. The water content of the pressed pepper raw material is lower than the range, the retention rate of piperine in the pepper raw material after the extraction of the essential oil is reduced, the quality of the subsequently prepared pepper resin product is influenced, the water content is higher than the range, the extraction speed of the essential oil is slow, the efficiency is low, and the industrial large-scale production efficiency is influenced.
Preferably, the freezing is carried out at-10-5 ℃ for 8-12h. Freezing at a temperature above this range increases the yield of pepper essential oil, which leads to a decrease in the yield of essential oil.
Preferably, the temperature of the pepper raw material is kept between-10 ℃ and 5 ℃ during the tabletting process. More preferably, the temperature is from-10 to-5 ℃.
During the tabletting process, cooling liquid with the temperature of-10 to 5 ℃ is preferably introduced to ensure the temperature of the pepper raw material. More preferably, the cooling liquid with the temperature of minus 10 to minus 5 ℃ is introduced.
Preferably, the thickness of the pellet is 0.3 to 0.5mm.
The above-mentioned compressed tablets can be compressed using a tablet press.
In the method for extracting pepper essential oil, the extraction solvent used in the subcritical extraction is butane. Compared with other extraction solvents, the butane is more beneficial to improving the extraction effect of pepper essential oil and pesticide residues and reducing the amount of extracted piperine.
Preferably, the temperature of the subcritical extraction is 20-25 ℃, and the pressure is 0.55-0.60MPa.
The invention discovers that the subcritical butane extraction temperature and pressure can influence the content of piperine in the obtained pepper oil and the pesticide residue of the extracted pepper raw material. The subcritical extraction temperature and pressure are higher than the above ranges, so that the piperine content in the obtained pepper oil is obviously improved, the content of the piperine in the extracted pepper raw material is reduced, and the quality of the extracted pepper product is influenced; the subcritical extraction temperature and pressure are lower than the ranges, so that the extraction speed of the essential oil is low, the efficiency is low, and the industrial large-scale production cannot be realized.
Preferably, the subcritical extraction is carried out 2-3 times, and each extraction time is 0.5-1.5h.
After subcritical extraction, pepper oil is obtained by filtration and evaporation.
In the method for extracting the pepper essential oil, the pressure of the molecular distillation is 1000-2000Pa, and the heating temperature is 75-80 ℃. The distillation efficiency of the essential oil is too low due to too high pressure and too low temperature of molecular distillation, the essential oil is difficult to be effectively separated from non-volatile components, and the pepper essential oil is too violently volatilized and cannot be condensed in time due to too low pressure and too high temperature, so that the yield of the essential oil is remarkably reduced.
In the above method, the collected molecular distillation light phase is the pepper essential oil.
In the above method, the residual pepper raw material after subcritical extraction of pepper oil can be used for preparing pepper oleoresin.
Production practices prove that the method for extracting the pepper essential oil has higher yield of the pepper essential oil, the content of piperine in the prepared molecular distillation heavy phase is less than or equal to 1 percent, and pesticide residues in pepper raw materials after the pepper oil (subcritical extraction) is extracted are less than or equal to 0.1ppm.
Wherein the pesticide is chlorpyrifos or metalaxyl.
The invention also provides the pepper essential oil prepared by the method for extracting the pepper essential oil.
The invention has the beneficial effects that: the invention provides a method for extracting piperine, which can ensure that the piperine is less extracted and reduce the loss of the piperine while ensuring the higher extraction yield of the piperine, thereby obviously improving the content of the piperine in pepper raw materials after the extraction of the piperine; the extraction method can also effectively remove pesticide residues in the pepper raw material, and ensure low pesticide residues in the pepper raw material after the pepper essential oil is extracted. In addition, the method also has the characteristics of convenient operation and industrial production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
This example provides a method for extracting pepper essential oil, which comprises the following steps:
1. tabletting: storing 30kg of pepper at-10 ℃ for 10h, tabletting by using a tabletting machine, introducing cooling liquid during tabletting, wherein the temperature of the cooling liquid is-10 ℃, the thickness of the pressed pepper is detected to be 0.4mm, and the water content in the pepper raw material is detected to be 16.01%;
2. subcritical extraction: putting 30kg of the pressed pepper raw material prepared in the step 1 into subcritical equipment, adding butane according to a material-liquid ratio of 1;
3. molecular distillation: and (3) putting the subcritical pepper oil obtained in the step (2) into a molecular distillation device, and distilling at 79 ℃ and 1250Pa to obtain 1200g of pepper essential oil and 1800g of molecular distillation heavy phase.
The calculated yield of the pepper essential oil in the method is 92.38 percent.
The subcritical pepper oil, the pepper essential oil and the pepper raw material extracted from the pepper oil prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content is detected according to GBT 17528-2009 piperine content determination high performance liquid chromatography. The results show that the content of piperine in the subcritical pepper oil is 0.55%, and the content of piperine in the pepper raw material after pepper oil extraction is 5.69%.
2. And (3) pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results showed that the content of chlorpyrifos residue in the pepper raw material after pepper oil extraction was 0.065ppm and the content of metalaxyl residue was 0.033ppm.
Example 2
This example provides a method for extracting pepper essential oil, which comprises the following steps:
1. tabletting: storing 30kg of pepper at-5 ℃ for 8h, tabletting by using a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of the cooling liquid at-5 ℃, measuring the thickness of the pressed pepper at 0.45mm, and measuring the water content in the pepper raw material at 18.33%.
2. Subcritical extraction: putting 30kg of the pressed pepper raw material prepared in the step 1 into subcritical equipment, adding butane according to the material-liquid ratio of 1.
3. Molecular distillation: putting 2.85kg of subcritical pepper oil obtained in step 2 into a molecular distillation device, distilling at 76 deg.C and 1650Pa to obtain 1168g of pepper essential oil, and 1782g of molecular distillation heavy phase.
The yield of pepper essential oil in the above process was calculated to be 91.52%.
The subcritical pepper oil, the pepper essential oil and the pepper raw material extracted from the pepper oil prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content is detected according to GBT 17528-2009 piperine content determination high performance liquid chromatography. The results show that the content of piperine in the subcritical pepper oil is 0.75%, and the content of piperine in the pepper raw material after pepper oil extraction is 5.66%.
2. And (3) pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results show that the chlorpyrifos residue in the pepper raw material after pepper oil extraction is 0.043ppm, and the metalaxyl residue is 0.023ppm.
Comparative example 1
The present comparative example provides a method for extracting pepper essential oil, comprising the steps of:
1. tabletting: storing 30kg of pepper at 10 ℃ for 10h, tabletting by using a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of the cooling liquid to be 10 ℃, measuring the thickness of the pepper after tabletting to be 0.4mm, and measuring the water content in the pepper raw material to be 16.52%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into subcritical equipment, extracting for 2 times at the temperature of 22 ℃ under the pressure of 0.56MPa, filtering for 1 hour each time, and evaporating to obtain 2.6kg of subcritical pepper oil.
3. Molecular distillation: 2.6kg of subcritical pepper oil obtained in the step 2 is put into a molecular distillation device and distilled under the conditions of 79 ℃ and 1250Pa to obtain 864g of pepper essential oil and 1736g of molecular distillation heavy phase.
The yield of pepper essential oil in the above method was calculated to be 66.5%, which is seen in the lower yield of essential oil due to volatilization of essential oil caused by higher temperature during tabletting.
Comparative example 2
The comparative example provides a method for extracting pepper essential oil, comprising the following steps:
1. tabletting: storing 30kg of pepper at-10 deg.C for 10h, tabletting with a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of cooling liquid at-10 deg.C, measuring the thickness of the pressed pepper at 0.4mm, and measuring the water content in pepper raw material at 11.03%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into subcritical equipment, extracting for 2 times at the temperature of 22 ℃ under the pressure of 0.56MPa, filtering for 1 hour each time, and evaporating to obtain 3.2kg of subcritical pepper oil.
3. Molecular distillation: putting 3.2kg of subcritical pepper oil obtained in step 2 into a molecular distillation device, and distilling at 79 ℃ under 1250Pa to obtain 1222g of pepper essential oil and 2015g of molecular distillation heavy phase.
The calculated yield of the pepper essential oil in the method is 92.38 percent.
The subcritical pepper oil, the pepper essential oil and the pepper raw material extracted from the pepper oil prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content was determined according to "high performance liquid chromatography for determining GBT 17528-2009 piperine content". The results showed that the content of piperine in the subcritical pepper oil was 8.31%, and the content of piperine in the pepper raw material after pepper oil extraction was 4.73%. Therefore, the insufficient moisture content in the pepper raw material can cause excessive extracted piperine, and further cause the content of the piperine in the product prepared from the pepper raw material after the essential oil is extracted to be reduced.
2. And (3) pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results show that the residue of chlorpyrifos in the pepper raw material after pepper oil extraction is 0.063ppm and the residue of metalaxyl is 0.030ppm.
Comparative example 3
The present comparative example provides a method for extracting pepper essential oil, comprising the steps of:
1. tabletting: storing 30kg of pepper at-10 deg.C for 10h, tabletting with a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of cooling liquid at-10 deg.C, measuring the thickness of the pressed pepper at 0.4mm, and measuring the water content in pepper raw material at 16.83%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into subcritical equipment, extracting for 2 times under the conditions of 0.65MPa and 30 ℃, filtering and evaporating for 1 hour each time to obtain 3.5kg of subcritical pepper oil.
3. Molecular distillation:
and 3.5kg of subcritical pepper oil obtained in the step 2 is put into a molecular distillation device and distilled under the conditions of 79 ℃ and 1250Pa to obtain 1228g of pepper essential oil and 2272g of molecular distillation heavy phase.
The calculated yield of pepper essential oil in the above method is 94.53%. The subcritical pepper oil, the pepper essential oil and the pepper raw material extracted from the pepper oil prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content was determined according to "high performance liquid chromatography for determining GBT 17528-2009 piperine content". The results show that the content of piperine in the subcritical pepper oil is 13.35%. Due to the over-high subcritical extraction pressure and temperature, the piperine is extracted more, which leads to the reduction of the piperine content of the product prepared from the pepper raw material after the extraction of essential oil.
2. And (3) pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results showed that the content of chlorpyrifos residue in the pepper raw material after pepper oil extraction was 0.036ppm and the content of metalaxyl residue was 0.012ppm.
Comparative example 4
The present comparative example provides a method for extracting pepper essential oil, comprising the steps of:
1. tabletting: storing 30kg of pepper at-10 deg.C for 10h, tabletting with a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of cooling liquid at-10 deg.C, measuring the thickness of the pressed pepper at 0.4mm, and measuring the water content in pepper raw material at 16.75%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into a subcritical device, extracting for 2 times under the conditions of 0.45MPa and 15 ℃, wherein each time is 1 hour, and filtering and evaporating to obtain 2.0kg of subcritical pepper oil.
3. Molecular distillation: 2.0kg of subcritical pepper oil obtained in the step 2 is put into a molecular distillation device and distilled under the conditions of 79 ℃ and 1250Pa to obtain 800g of pepper essential oil and 1200g of molecular distillation heavy phase.
The calculated yield of the pepper essential oil in the method is 41.16 percent.
The subcritical pepper oil, the pepper essential oil and the pepper raw material extracted from the pepper oil prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content is detected according to GBT 17528-2009 piperine content determination high performance liquid chromatography. The results show that the content of piperine in the subcritical pepper oil is 0.31%, and the content of piperine in the pepper raw material after pepper oil extraction is 5.46%.
2. And (3) pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results showed that the content of chlorpyrifos residue in the pepper raw material after pepper oil extraction was 0.233ppm and the content of metalaxyl residue was 0.351ppm. Because the subcritical extraction pressure and temperature are too low, the yield of the extracted essential oil is low, the extraction efficiency is low, and the pesticide residue index in the extracted pepper is unqualified.
Comparative example 5
The present comparative example provides a method for extracting pepper essential oil, comprising the steps of:
1. tabletting: storing 30kg of pepper at-10 ℃ for 10h, tabletting by using a tabletting machine, introducing cooling liquid during tabletting, detecting the temperature of the cooling liquid to be-10 ℃, and detecting the thickness of the pepper after tabletting to be 0.4mm and the water content in the pepper raw material to be 15.89%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into a subcritical device, extracting for 2 times at the temperature of 22 ℃ under the pressure of 0.56MPa, wherein each time is 1 hour, and filtering and evaporating to obtain 3kg of subcritical pepper oil.
3. Molecular distillation: and 3kg of subcritical pepper oil obtained in the step 2 is put into a molecular distillation device and distilled under the conditions of 70 ℃ and 2500Pa to obtain 750g of pepper essential oil and 2250g of molecular distillation heavy phase.
The yield of pepper essential oil in the above process was calculated to be 62.5%. Due to the excessively low molecular distillation temperature and the excessively high pressure, the yield of the pepper essential oil is significantly reduced compared to example 1, and more essential oil cannot be effectively extracted in the molecular distillation heavy phase.
Comparative example 6
The comparative example provides a method for extracting pepper essential oil, comprising the following steps:
1. tabletting: storing 30kg of pepper at-10 deg.C for 10h, tabletting with a tabletting machine, introducing cooling liquid during tabletting, measuring the temperature of cooling liquid at-10 deg.C, measuring the thickness of the pressed pepper at 0.4mm, and measuring the water content in the pepper raw material at 15.63%.
2. Subcritical extraction: and (2) putting 30kg of the pressed pepper raw material obtained in the step (1) into subcritical equipment, extracting for 2 times at the temperature of 22 ℃ under the pressure of 0.56MPa, filtering for 1 hour each time, and evaporating to obtain 3kg of subcritical pepper oil.
3. Molecular distillation: and 3kg of subcritical pepper oil obtained in the step 2 is put into a molecular distillation device and distilled under the conditions of 85 ℃ and 800Pa to obtain 810g of pepper essential oil and 1800g of molecular distillation heavy phase.
The calculated yield of the pepper essential oil in the method is 62.26 percent. Due to the fact that the molecular distillation temperature is too high and the pressure is too low, the weight loss rate in the molecular distillation step reaches 13%, and more essential oil cannot be condensed and lost due to too fast volatilization.
Comparative example 7
The present comparative example provides a method for extracting pepper essential oil, comprising the steps of:
1. tabletting: storing 30kg of pepper at-10 ℃ for 10h, tabletting by using a tabletting machine, introducing cooling liquid during tabletting, wherein the temperature of the cooling liquid is-10 ℃, the thickness of the pressed pepper is detected to be 0.4mm, and the water content in the pepper raw material is detected to be 16.01%;
2. supercritical extraction: putting 30kg of the pressed pepper raw material prepared in the step 1 into supercritical equipment, adding carbon dioxide according to a material-liquid ratio of 1;
3. molecular distillation: and (3) putting 5kg of supercritical pepper oil obtained in the step (2) into a molecular distillation device, and distilling at 79 ℃ and 1250Pa to obtain 1208g of pepper essential oil and 3756g of molecular distillation heavy phase.
The yield of pepper essential oil in the above process was calculated to be 93.01%.
The supercritical pepper oil, the pepper essential oil and the pepper raw material after pepper oil extraction prepared by the method are detected as follows:
1. detecting the content of piperine: the piperine content is detected according to GBT 17528-2009 piperine content determination high performance liquid chromatography. The results show that the content of piperine in the supercritical pepper oil is 15.51%, and the content of piperine in the pepper raw material after pepper oil extraction is 3.04%. In the supercritical extraction process, more piperine is extracted, which results in the reduction of piperine content in the product prepared from the pepper raw material after the extraction of essential oil
2. Pesticide residue detection: various pesticide residues were detected using a liquid phase mass spectrometer. The results show that the chlorpyrifos residue in the pepper raw material after the pepper oil extraction is 0.045ppm, and the metalaxyl residue is 0.031ppm.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for extracting pepper essential oil, comprising: performing subcritical extraction on the pepper raw material to obtain pepper oil, performing molecular distillation on the pepper oil, and collecting a light phase.
2. The method of claim 1, wherein the pepper raw material is frozen and then tabletted before the subcritical extraction, and the moisture content of the tabletted pepper raw material is 15-20%.
3. The method for extracting pepper essential oil as claimed in claim 2, wherein the freezing is at-10-5 ℃ for 8-12h.
4. The method for extracting pepper essential oil according to claim 3, wherein the temperature of the pepper raw material is maintained at-10 to 5 ℃ during the tabletting process.
5. The method for extracting pepper essential oil as claimed in any one of claims 2-4, wherein the thickness of the pressed sheet is 0.3-0.5mm.
6. The method for extracting pepper essential oil as claimed in any one of claims 1-5, wherein the extraction solvent used in the subcritical extraction is butane.
7. The method for extracting pepper essential oil according to claim 6, wherein the temperature of the subcritical extraction is 20-25 ℃ and the pressure is 0.55-0.60MPa.
8. The method for extracting pepper essential oil as claimed in claim 7, wherein the subcritical extraction is performed 2-3 times, each extraction time is 0.5-1.5h.
9. The method for extracting pepper essential oil according to any one of the claims 1-8, wherein the pressure of the molecular distillation is 1000-2000Pa and the heating temperature is 75-80 ℃.
10. A pepper essential oil prepared by the method for extracting pepper essential oil of any one of claims 1-9.
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