CN108967994B - Preparation method of pepper flavor substance - Google Patents
Preparation method of pepper flavor substance Download PDFInfo
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- CN108967994B CN108967994B CN201811159892.4A CN201811159892A CN108967994B CN 108967994 B CN108967994 B CN 108967994B CN 201811159892 A CN201811159892 A CN 201811159892A CN 108967994 B CN108967994 B CN 108967994B
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Images
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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- 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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/115—Natural spices, flavouring agents or condiments; Extracts thereof obtained by distilling, stripping, or recovering of volatiles
-
- 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
Abstract
The invention relates to the technical field of plant extraction, in particular to a method for extracting pepper flavor substances by taking fresh pepper with spikes as a main raw material. The invention pulping whole fresh pepper fruits, extracting pepper volatile flavor substances by a co-water distillation method, carrying out ultrasonic-microwave synergistic extraction on the extracted pepper pulp by using ethanol as a solvent, and concentrating and drying the extract to obtain non-exerted flavor substances. The method realizes complete extraction of pepper flavor substances, obviously improves the yield of pepper flavor substances, and the obtained pepper flavor substances are rich in nutrient substances such as polyphenol, piperine and the like. The method takes fresh pepper fruits as raw materials for extraction, reduces the working procedure of processing pepper into pepper, obviously reduces the production cost, and effectively avoids the adverse effect of the pepper processing procedure in the traditional process on the environment. The residual pepper pulp after extraction can also be used as the raw material of pepper sauce, thus fully utilizing pepper resources and being beneficial to promoting the upgrading of pepper industry.
Description
Technical Field
The invention relates to the technical field of plant extraction, and particularly relates to a preparation method of a pepper flavor substance.
Background
Pepper nigrum L is a perennial evergreen vine plant of the Piper genus of the family Piperaceae, is native to tropical rain forest of the western Hippocampus at West coast of India, has been cultivated as early as 2000, is an important spice crop in the world, and is homologous in medicine and food. The traditional Chinese medicine considers that the pepper is pungent, hot and nontoxic in taste, can warm the middle-jiao to dispel cold, promote qi circulation to relieve pain, and is suitable for treating cold excess of the middle-jiao, indigestion, abdominal psychroalgia, regurgitation emesis, diarrhea and dysentery, etc. In the medical industry, pepper can be used as stomachic, antipyretic and bronchial mucosa irritant, and can be used for treating dyspepsia, cold phlegm, cough, enteritis, bronchitis, common cold and rheumatism, and in the food industry, also can be used as antiseptic. The seed of fructus Piperis contains volatile oil, piperine, crude fat, crude protein, lignanoids, alkaloids, flavonoids, aromatic compounds, amides, etc. Wherein, the piperine is approved as a food additive by the Ministry of public health of the people's republic of China in 2004, and has significant adjuvant treatment and regulation effects on epilepsy, gastric ulcer, atherosclerosis, depression, immunity, brain function and the like. Researches in recent years show that pepper has activity in various aspects such as analgesia, sedation, anti-inflammation, anticonvulsion, bacteriostasis, disinsection, anticancer and the like, can be widely applied to the fields of modern pharmacy, smoking cessation, drug rehabilitation, military and the like after being modified by bioengineering, and has wide application and high economic value.
The pepper flavor substances comprise volatile flavor substances (mainly volatile oil) and nonvolatile flavor substances (mainly pepper spicy flavor substances), the volatile flavor substances can be extracted by steam distillation, the nonvolatile flavor substances are mainly prepared by extracting components such as color, aroma and taste in pepper by a solvent extraction method, and the obtained extract is subjected to processes such as filtration, solvent removal, drying and the like. The water, ether or ethanol extract of fructus Piperis has effects of killing tapeworm, deodorizing, antisepticizing and resisting oxidation.
At present, methods for extracting pepper flavor substances at home and abroad include a solvent extraction method, a Soxhlet extraction method, a microwave method, an ultrasonic method, a supercritical method and the like. Among them, the method for retaining the aroma and flavor components in pepper is supercritical, and the method has limitations: the piperine is largely crystallized at the extraction temperature, which causes complex extraction process and high extraction cost. In contrast, the solvent extraction process accelerated by the field effect is quick and convenient, and is particularly beneficial to the extraction and separation of the flavor components of the black pepper with higher polarity and higher content.
However, the existing pepper flavor substances are prepared by taking black pepper powder or white pepper powder as raw materials, fresh pepper fruits are peeled, dried and crushed in advance and then can be used for extraction, so that the production cost is high and the resource is wasted.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing pepper flavor substances. The preparation method provided by the invention realizes the complete extraction of pepper flavor substances, the yield of pepper nonvolatile flavor substances is high, the piperine content is higher, and the prepared flavor substances have enough piquancy, stronger aroma and better quality. The fresh pepper fruits are used as raw materials for extraction, so that the production cost is greatly reduced.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
the invention provides a preparation method of pepper flavor substances, which comprises the following steps:
step 1: pulping fresh fructus Piperis with water to obtain fructus Piperis pulp, and extracting by steam distillation to obtain oil and water slurry;
step 2: adding the water slurry obtained in the step (1) into an ethanol water solution, uniformly mixing, and performing ultrasonic-microwave synergistic extraction, concentration and drying to obtain a paste;
and step 3: collecting the oil in the step 1 and the paste in the step 2 to obtain pepper flavor substances.
According to the invention, fresh pepper fruits are used as raw materials to extract pepper flavor substances, a steam distillation method and an ultrasonic-microwave synergistic extraction method are combined to completely extract the pepper flavor substances, the yield of the pepper flavor substances is obviously improved, and the obtained pepper flavor substances are rich in volatile and non-volatile nutrient substances. In the obtained pepper flavor substances, the oily substances are mainly 3-carene, limonene, caryophyllene and other volatile flavor substances, and the paste is mainly polyphenol substances, piperine and other non-volatile flavor substances.
In some embodiments, the steam distillation extraction in step 1 uses a collector to collect volatile flavor substances, and the collector is made of glass, so that steam can pass through the collector conveniently, and the condensed volatile flavor substances can be collected. The condensing pipe needs to be filled with condensate, so that the temperature of the condensing pipe is kept at 0-8 ℃, and volatile flavor substances can be conveniently and timely cooled. The used utensils are made of heat-resistant glass, the joints are ground, and vaseline is coated before the utensils are used to keep the whole distillation process sealed, so that the loss of volatile flavor substances is prevented. The distillation time is measured after the pepper pulp is boiled, and the total content of the collected oily volatile flavor substances is not increased any more. And centrifuging to remove water in the distilled pepper pulp, wherein the centrifugation parameter is 3000-5000 rpm, and centrifuging for 3-8 min. The volatile flavor substances are preferably stored in a refrigerator at a temperature below 4 ℃ in a sealed manner to prevent volatilization.
The method comprises the following steps of 1, preparing pepper pulp, and extracting by adopting a steam distillation method. In some embodiments, the pepper paste is prepared by: selecting fresh pepper fruits without diseases and insect pests as raw materials, adding water according to the mass ratio of 1: 1-2 of the material liquid, and grinding by using a pulping machine to obtain pepper pulp. Wherein, the fresh pepper with spike is the fresh pepper with stem.
In some embodiments, the steam distillation extraction conditions are: adding water into the pepper pulp, heating and boiling, and distilling and extracting for 3-4 h. In some embodiments, the mass ratio of pepper paste to water is 1: 3 to 6.
In the step 1 of the invention, volatile oily substances and nonvolatile water serous fluid are respectively obtained after the pepper serous fluid is distilled and extracted by steam. In the step 2 of the invention, the water slurry is subjected to ultrasonic-microwave synergistic extraction.
In some embodiments, in the ultrasonic-microwave synergistic extraction in the step 2, the power of the ultrasonic wave is 50W, and the frequency is 25-35 KHz; the microwave power is 550-700W, the microwave frequency is 2500-3500 MHz, the extraction time is 15-30 min, and the extraction temperature is 60-80 ℃. In some embodiments, in the ultrasonic-microwave synergistic extraction in the step 2, the power of the ultrasonic wave is 50W, and the frequency is 28 KHz; the microwave power is 550, the microwave frequency is 3000MHz, the extraction time is 20min, and the extraction temperature is 70 ℃.
In some embodiments, the mass ratio of the fresh pepper fruits to the water in the step 1 is 1: 4-10. In some embodiments, the mass ratio of the fresh pepper fruits to water in step 1 is 1: 6. In some embodiments, the mass ratio of the fresh pepper fruits to water in step 1 is 1: 8.
In some embodiments, the volume fraction of ethanol in the ethanol aqueous solution in the step 2 is 70-95%. In some embodiments, the volume fraction of ethanol in the aqueous ethanol solution of step 2 is 95%.
In some embodiments, the concentration in step 2 is specifically performed for 10 to 70min under the conditions of a vacuum degree of 0.1 to 0.9MPa and a temperature of 35 to 60 ℃. In some embodiments, the concentration in step 2 is performed for 20-40 min under the conditions of a vacuum degree of 0.3-0.5 MPa and a temperature of 40-50 ℃.
The invention also provides the pepper flavor substance prepared by the method.
According to the invention, fresh pepper fruits are used as raw materials to extract pepper flavor substances, a steam distillation method and an ultrasonic-microwave synergistic extraction method are combined to completely extract the pepper flavor substances, the yield of the pepper flavor substances is obviously improved, and the obtained pepper flavor substances have sufficient pungency, stronger aroma and better quality. Meanwhile, fresh pepper fruits are used as raw materials for extraction, so that the processing procedures of pepper are reduced, and the production cost is greatly reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a total ion flow diagram of the volatile flavors in the pepper flavor of example 1 of the present invention;
fig. 2 is a total ion flow diagram of the volatile flavors in the pepper flavor of comparative example 1.
Detailed Description
The invention discloses a preparation method of pepper flavor substances, and the method can be realized by appropriately improving process parameters by taking the contents of the pepper flavor substances as reference. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
The invention is further illustrated by the following examples:
example 1
Raw materials: 10 parts of fresh pepper with spike, 60 parts of deionized water and 350 parts of 95% edible alcohol.
The preparation method comprises the following steps:
(1) preparing pepper paste: selecting fresh pepper fruits without plant diseases and insect pests and with spikes as raw materials, wherein part of the fresh pepper fruits are changed into yellow, adding 10 parts of deionized water into 10 parts of the fresh pepper fruits, and grinding the mixture by a grinder to ensure that no obvious particles or spikes are contained in the pulp;
(2) steam distillation: adding 50 parts of water into 10 parts of pepper pulp, heating and boiling, and arranging a collector and a condenser pipe, wherein the connection part is kept sealed; after 3h of distillation, the oily pepper flavor was collected and dehydrated with anhydrous sodium sulfate to obtain an oil and an aqueous slurry, wherein the oily pepper flavor was preserved in a brown glass bottle under sealed conditions.
(3) Collecting pepper water slurry, centrifuging at 4000rpm at 10 deg.C for 5min to remove most water; adding 350 parts of 95% edible alcohol into the water slurry after centrifugation in the step (2);
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/28KHz, microwave power: 550W, microwave frequency: 3000MHz, 20min of extraction time and 70 ℃ of extraction temperature;
(5) filtering, rapidly filtering visible substances such as fructus Piperis powder by vacuum filtration, wherein the aperture of the filter membrane is less than 0.15mm, and collecting the filtrate;
(6) removing the solvent by adopting vacuum low-temperature rotary concentration, wherein the vacuum degree is controlled to be 0.05MPa, and the temperature is controlled to be 40 ℃;
(7) drying, vacuum drying at vacuum degree of 0.08MPa and temperature of 50 deg.C to obtain fructus Piperis extract;
(8) the pepper oil and pepper extract were collected to obtain 1.6 parts pepper flavor substance.
Example 2
Raw materials: 10 parts of fresh pepper with spike, 80 parts of deionized water and 500 parts of 95% edible alcohol.
The preparation method comprises the following steps:
(1) preparing pepper paste: selecting fresh pepper fruits without plant diseases and insect pests and with spikes as raw materials, wherein part of the fresh pepper fruits are changed into yellow, adding 20 parts of deionized water into 10 parts of the fresh pepper fruits, and grinding the mixture by a grinder to ensure that no obvious particles or spikes are contained in the pulp;
(2) steam distillation: adding 60 parts of water into 10 parts of pepper pulp, heating and boiling, and putting the pepper pulp on a receiver and a condenser pipe, wherein the joint is kept sealed; after distillation for 4h, the oily pepper flavor was collected and dehydrated with anhydrous sodium sulfate to obtain an oil and an aqueous slurry, wherein the oily pepper flavor was preserved in a brown glass bottle under sealed conditions.
(3) Collecting pepper water slurry, centrifuging at 10 deg.C under 5000rpm for 3min to remove most water; adding 500 parts of 95% edible alcohol into the water slurry after centrifugation in the step (2);
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/30KHz, microwave power: 600W, microwave frequency: 2500MHz, synergistic extraction for 30 min;
(5) filtering, rapidly filtering visible substances such as fructus Piperis powder by vacuum filtration, wherein the aperture of the filter membrane is less than 0.15mm, and collecting the filtrate;
(6) removing the solvent by adopting vacuum low-temperature rotary concentration, wherein the vacuum degree is controlled to be 0.05MPa, and the temperature is controlled to be 45 ℃;
(7) drying, vacuum drying at vacuum degree of 0.08MPa and temperature of 50 deg.C to obtain fructus Piperis extract;
(8) the pepper oil and pepper extract were collected to obtain 1.6 parts pepper flavor substance.
Comparative example 1
In the comparative example, the pepper flavor substances are extracted from the dried pepper fruits, and the preparation method comprises the following steps:
(1) drying fresh pepper fruits with spikes until the water content is less than 12% to obtain dried pepper fruits, and crushing and sieving the dried pepper fruits until the granularity reaches 40 meshes to obtain pepper powder;
(2) and (3) carrying out co-water distillation on 10 parts of pepper powder by 500 parts of deionized water for 4h, collecting oily pepper flavor substances, and removing water by using anhydrous sodium sulfate to obtain oily substances and water slurry, wherein the oily pepper flavor substances are stored in a brown glass bottle in a sealed manner.
(3) Collecting pepper water slurry, centrifuging at 4000rpm at 10 deg.C for 5min to remove most water; adding 350 parts of 95% edible alcohol into the water slurry after centrifugation in the step (2);
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 300W, microwave frequency: 2450MHz, and performing synergistic extraction for 10 min.
The other steps are the same as in example 1.
Comparative example 2
Raw materials: 10 parts of fresh pepper with spike, 60 parts of deionized water and 350 parts of 95% edible alcohol.
The preparation method is different from the step (4) of the example 1, and the other conditions are the same;
wherein, the step (4): ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 300W, microwave frequency: 2450MHz, and synergistic extraction for 20 min.
Example 3 detection assay of volatile flavors in Pepper flavors
GCMS detection analysis is carried out on pepper flavor substance samples prepared in example 1 and comparative example 1, wherein a total ion flow diagram of pepper flavor substances prepared in example 1 is shown in figure 1, a total ion flow diagram of pepper flavor substances prepared in comparative example 1 is shown in figure 2, and the quantitative analysis results of the samples are shown in table 1.
TABLE 1 relative content of flavor (%) -of different pepper samples
As can be seen from the results of FIGS. 1-2, the abundance response of the sample in FIG. 1 reaches 8X 107The abundance response of the sample of FIG. 2 is 1.4X 107Meanwhile, the number of chromatographic peaks in fig. 1 is much higher than that in fig. 2. Wherein, the higher the response value is, the larger the peak area is, and the larger the relative percentage content of the flavor substances is; the greater the number of chromatographic peaks, the greater the number of flavor compounds. The results shown in fig. 1-2 and table 1 show that the types and contents of the volatile flavors in the pepper flavor prepared in example 1 of the present invention are significantly better than those in comparative example 1.
Example 4 Effect of different extraction methods on the content of non-volatile flavor substances
This example compares the yield of non-volatile flavors in the pepper flavors and the total polyphenol and piperine content in the non-volatile flavors obtained by the following extraction methods, and the results are shown in table 2, and compares the extraction costs of the several methods, and the results are shown in table 3.
Hot reflux extraction method: 10 parts of pepper sample is filled in a flask, 100 parts of ethanol with the volume ratio of 95% is added for extraction, the solution is kept boiling in a water bath at 85 ℃, a condensation pipe is connected to the flask, cooling liquid is connected to the condensation pipe, the cooling liquid is conveyed through a cooling circulating pump, steam generated by the boiling solution of the cooling liquid is condensed into the flask through the condensation pipe, the steps are repeated, reflux extraction is carried out for 3 hours, finally the solution subjected to reflux extraction is concentrated through a rotary evaporator, the solvent is recovered, and finally the concentrated solution is subjected to vacuum drying to obtain the nonvolatile flavor substance.
Microwave extraction method: 10 parts of pepper sample is filled in a flask, 100 parts of ethanol with the volume ratio of 95% is added for extraction, the microwave power is 300W, the temperature of the solution is kept at 80-90 ℃, a condensation pipe is connected to the flask, cooling liquid is connected to the condensation pipe, the cooling liquid is conveyed through a cooling circulating pump, steam generated by boiling solution of the cooling liquid is condensed into the flask through the condensation pipe, the steps are repeated, microwave extraction is carried out for 0.5h, the finally extracted solution is concentrated through a rotary evaporator, the solvent is recovered, and the concentrated solution is finally subjected to vacuum drying to obtain the nonvolatile flavor substance.
An ultrasonic extraction method comprises the following steps: 10 parts of pepper sample is filled in a flask, 100 parts of ethanol with the volume ratio of 95% is added for extraction, ultrasonic extraction is used in a water bath at the temperature of 30 ℃, a condensation pipe is connected to the flask, cooling liquid is connected to the condensation pipe, the cooling liquid is conveyed through a cooling circulating pump, steam generated by boiling solution of the cooling liquid is condensed into the flask through the condensation pipe, the operation is repeated, ultrasonic extraction is carried out for 0.5h, finally extracted solution is concentrated through a rotary evaporator, solvent is recovered, and finally the concentrated solution is dried in vacuum to obtain the nonvolatile flavor substance.
The content of nonvolatile flavor substances is shown in Table 2.
TABLE 2 Effect of different extraction methods on the content of non-volatile flavour substances
TABLE 3 comparison of extraction time and cost
The results show that the yield of pepper flavor substances is obviously higher than that of a hot reflux extraction method, a microwave extraction method, an ultrasonic extraction method and the methods of comparative examples 1-2, and the content of the obtained nonvolatile flavor substances is also obviously higher. Meanwhile, compared with other methods, the extraction method disclosed by the invention has the advantages that the raw materials required for obtaining 100g of pepper flavor substances are less, the power consumption is low, and the time consumption is shorter.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The preparation method of the pepper flavor substance is characterized by comprising the following steps:
step 1: pulping fresh fructus Piperis with water to obtain fructus Piperis pulp, and extracting by steam distillation to obtain oil and water pulp;
step 2: adding the water slurry obtained in the step (1) into an ethanol water solution, uniformly mixing, and performing ultrasonic-microwave synergistic extraction, concentration and drying to obtain a paste;
and step 3: collecting the oil substance in the step 1 and the paste substance in the step 2 to obtain pepper flavor substances;
in the ultrasonic-microwave synergistic extraction, the power of ultrasonic is 50W, and the frequency is 25-35 KHz; the microwave power is 550-700W, the microwave frequency is 2500-3500 MHz, the extraction time is 15-30 min, and the extraction temperature is 60-80 ℃;
and 2, the volume fraction of the ethanol in the ethanol aqueous solution in the step 2 is 70-95%.
2. The preparation method according to claim 1, wherein in the ultrasonic-microwave synergistic extraction in the step 2, the power of the ultrasonic wave is 50W, and the frequency is 28 KHz; the microwave power is 550W, the microwave frequency is 3000MHz, the extraction time is 20min, and the extraction temperature is 70 ℃.
3. The preparation method of claim 1, wherein the mass ratio of the fresh pepper fruits to the water in the step 1 is 1: 4-10.
4. The preparation method as claimed in claim 3, wherein the mass ratio of the fresh pepper fruits to the water in the step 1 is 1: 6.
5. A pepper-flavor substance prepared by the preparation method of any one of claims 1 to 4.
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