CN108967994A - A kind of preparation method of pepper flavor substance - Google Patents

Abstract

The present invention relates to technical field of plant extraction, specifically the method to extract pepper flavor substance as primary raw material with fringe pepper fresh fruit.Whole fringe pepper fresh fruit is beaten by the present invention, extracts pepper volatile flavor substance with distilling with water method, the pepper slurry after extraction is carried out Ultrasonic-microwave synergistic extraction by solvent of ethyl alcohol, extract liquor is concentrated, drying obtains not performance property flavor substance.The method achieve the complete extractions to pepper flavor substance, hence it is evident that improves the yield of pepper flavor substance, gained pepper flavor substance is rich in nutriments such as polyphenol, piperines.This method is extracted using pepper fresh fruit as raw material, reduces the process that pepper is processed as pepper powder, hence it is evident that is reduced production cost, is simultaneously effective avoided adverse effect of the pepper powder processing program to environment in traditional handicraft.Remaining pepper slurry is alternatively arranged as the raw material of pepper sauce after extraction, is sufficiently used pepper resource, may advantageously facilitate pepper industrial upgrading.

Description

A kind of preparation method of pepper flavor substance

technical field

The invention relates to the technical field of plant extraction, in particular to a method for preparing pepper flavor substances.

Background technique

Pepper (Piper nigrum L.) is a perennial evergreen vine belonging to the family Piperaceae. Pepper is native to the tropical rainforest of the Western Ghats on the west coast of India. It has been cultivated as early as 2000 years ago. It is an important spice crop in the world. Eat the same origin. Traditional Chinese medicine believes that pepper is pungent, hot in nature, and non-toxic. It can warm the middle and dispel cold, promote qi and relieve pain. In the medical industry, pepper can be used as a stomachic agent, antipyretic and bronchial mucosal stimulant, etc., to treat indigestion, cold phlegm, cough, enteritis, bronchitis, cold and rheumatism, etc. In addition, it is also used in the food industry. Used as a preservative. Pepper seeds contain volatile oil, piperine, crude fat, crude protein, lignans, alkaloids, flavonoids, aromatic compounds and amides. Among them, piperine was approved as a food additive by the Ministry of Health of the People's Republic of China in 2004, focusing on epilepsy, gastric ulcer, atherosclerosis, depression, immunity, and brain function. Studies in recent years have shown that pepper is active in many aspects such as analgesia, sedation, anti-inflammation, anti-convulsion, antibacterial, insecticide, and anti-cancer. And military and other fields, with wide application and high economic value.

Pepper flavor substances include volatile flavor substances (mainly volatile oil) and non-volatile flavor substances (mainly pepper spicy substances), volatile flavor substances can be extracted by steam distillation, and non-volatile flavor substances are mainly obtained by The solvent extraction method extracts the color, aroma, taste and other components in the pepper, and the obtained extract is obtained by filtering, removing the solvent, drying and other processes. Water, ether or ethanol extracts of pepper have tapeworm-killing, deodorizing, antiseptic and antioxidant properties.

At present, the methods for extracting pepper flavor substances at home and abroad include solvent extraction, Soxhlet extraction, microwave method, ultrasonic method and supercritical method. Among them, the best method for retaining the aromatic and taste components in pepper is the supercritical method, but this method also has limitations: a large amount of piperine crystallizes at its extraction temperature, resulting in complicated extraction process and high extraction cost. In contrast, the field-effect-accelerated solvent extraction process is quick and convenient, and it is especially beneficial to the extraction and separation of higher polarity and higher content of black pepper flavor components.

However, the preparation of existing pepper flavor substances all use black pepper powder or white pepper powder as raw materials, and the fresh fruit of pepper must be peeled, dried and crushed in advance before being used for extraction, resulting in high production costs and waste of resources. Moreover, after the above-mentioned series of After treatment, the original active substances such as polyphenols in the fresh pepper fruit are basically lost and cannot be fully utilized.

Contents of the invention

In view of this, the object of the present invention is to provide a preparation method of pepper flavor substances. The preparation method provided by the invention realizes the complete extraction of pepper flavor substances, and the yield of non-volatile flavor substances of pepper is high, and the content of piperine in it is also high, and the prepared flavor substances have sufficient spicy taste and stronger aroma. The quality is better. The fresh pepper fruit is used as the raw material for extraction, which greatly reduces the production cost.

In order to realize the purpose of the present invention, the present invention adopts following technical scheme:

The present invention provides a kind of preparation method of pepper flavor substance, comprises the following steps:

Step 1: Take fresh pepper fruit and add water to make a pulp to make pepper pulp, extract by steam distillation to obtain oily substance and water slurry;

Step 2: Take the water slurry in step 1, add ethanol aqueous solution and mix evenly, and extract through ultrasonic-microwave synergy, concentrate and dry to obtain a paste;

Step 3: Collect the oily substance described in step 1 and the paste described in step 2 to obtain pepper flavor substances.

The present invention extracts pepper flavor substances from fresh pepper fruits, and combines steam distillation and ultrasonic-microwave cooperative extraction to completely extract pepper flavor substances, and significantly improves the yield of pepper flavor substances, and the obtained pepper flavor substances are rich Contains volatile and non-volatile nutrients. Among the obtained pepper flavor substances, the oily substances are mainly volatile flavor substances such as 3-carene, limonene, and caryophyllene, and the paste-like substances are mainly nonvolatile flavor substances such as polyphenols and piperine.

In some specific embodiments, the water vapor distillation extraction in step 1 uses a collector to collect volatile flavor substances, and the collector is made of glass, which not only facilitates the passage of water vapor, but also collects condensed volatile flavor substances. Condensate should be fed into the condenser tube to keep the temperature of the condenser tube at 0-8°C to facilitate timely cooling of volatile flavor substances. The utensils used are all heat-resistant glass, and the joints are all ground. Before use, apply Vaseline to keep the whole distillation process sealed to prevent the loss of volatile flavor substances. The distillation time starts after the pepper pulp boils, and the total content of the collected oily volatile flavor substances no longer increases. The moisture in the distilled pepper pulp is removed by centrifugation, the centrifugation parameters are 3000-5000rpm, and the centrifugation is 3-8min. The storage of volatile flavor substances should be sealed and stored in a refrigerator below 4°C to prevent volatilization.

In step 1 of the present invention, pepper pulp is prepared first, and then steam distillation is used for extraction. In some specific embodiments, the preparation method of pepper pulp is as follows: select fresh peppers with ears free of pests and diseases as raw materials, add water according to the mass ratio of material to liquid at a ratio of 1:1 to 2, and grind with a refiner to obtain Pepper pulp. Wherein, the fresh peppery fruit with ears is the fresh peppery fruit with fruit stem preserved.

In some embodiments, the steam distillation extraction condition is as follows: adding water to the pepper pulp, heating and boiling, and distillation extraction for 3-4 hours. In some embodiments, the mass ratio of pepper pulp to water is 1:3-6.

In Step 1 of the present invention, volatile oily matter and non-volatile water slurry are respectively obtained after steam distillation and extraction of pepper pulp. In step 2 of the present invention, ultrasonic-microwave cooperative extraction is performed on the water slurry.

In some embodiments, in the ultrasonic-microwave cooperative extraction described in step 2, the ultrasonic power is 50W, the frequency is 25-35KHz; the microwave power is 550-700W, the microwave frequency is 2500-3500MHz, and the extraction time is 15-30min. The extraction temperature is 60-80°C. In some specific embodiments, in the ultrasonic-microwave cooperative extraction described in step 2, the ultrasonic power is 50W, the frequency is 28KHz; the microwave power is 550, the microwave frequency is 3000MHz, the extraction time is 20min, and the extraction temperature is 70°C.

In some embodiments, the mass ratio of fresh pepper fruit to water in step 1 is 1:4-10. In some specific embodiments, the mass ratio of the fresh fruit of pepper described in step 1 to water is 1:6. In some specific embodiments, the mass ratio of the fresh fruit of pepper described in step 1 to water is 1:8.

In some embodiments, the volume fraction of ethanol in the aqueous ethanol solution in step 2 is 70-95%. In some specific embodiments, the volume fraction of ethanol in the aqueous ethanol solution in step 2 is 95%.

In some embodiments, the concentrating in step 2 is specifically concentrating for 10-70 min at a vacuum degree of 0.1-0.9 MPa and a temperature of 35-60°C. In some specific embodiments, the concentrating in step 2 is specifically concentrating for 20-40 min under the conditions of a vacuum degree of 0.3-0.5 MPa and a temperature of 40-50°C.

The present invention also provides the pepper flavor substance prepared by the above method.

The invention uses fresh pepper fruit as raw material to extract pepper flavor substances, combined with steam distillation method and ultrasonic-microwave cooperative extraction method, completely extracts pepper flavor substances, and obviously improves the yield of pepper flavor substances, and the obtained pepper flavor substances are hot and spicy. Full flavor, stronger aroma and better quality. At the same time, the fresh pepper fruit is used as the raw material for extraction, which reduces the processing steps of the pepper and greatly reduces the production cost.

Description of drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings that are required in the description of the embodiments or the prior art.

Fig. 1 is the total ion flow diagram of the volatile flavor substances in the pepper flavor substances of Example 1 of the present invention;

Fig. 2 is the total ion chromatogram of the volatile flavor substances in the pepper flavor substances of Comparative Example 1.

Detailed ways

The invention discloses a method for preparing a pepper flavor substance, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The method and application of the present invention have been described through preferred embodiments, and the relevant personnel can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention to realize and Apply the technology of the present invention.

The disclosed embodiments are described to enable any person skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention will not 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 used in the present invention are all common commercially available products, which can be purchased in the market.

Below in conjunction with embodiment, further set forth the present invention:

Example 1

Raw materials: 10 parts of fresh pepper with spikes, 60 parts of deionized water, 350 parts of 95% edible alcohol.

Preparation:

(1) Preparation of pepper pulp: select the fresh fruit of pepper with ears without damage by diseases and insect pests as raw material, and some of the colors in the fresh fruit turn yellow, get 10 parts of fresh pepper fruit and add 10 parts of deionized water, grind with a refiner, and make it in the slurry No obvious grains or stalks;

(2) Steam distillation: add 50 parts of water to 10 parts of pepper pulp, heat to boil, and then collect the collector and condenser, and keep the joints sealed; after 3 hours of distillation, collect the oily pepper flavor substances, and remove them with anhydrous sodium sulfate. Remove moisture to obtain oily substance and water slurry, wherein the pepper flavor substance of the oily substance is sealed and preserved in a brown glass bottle.

(3) Collect the pepper water slurry, remove most of the water by centrifuging at 10° C. for 5 min at 4000 rpm; add 350 parts of 95% edible alcohol to the centrifuged water slurry in step (2);

(4) Ultrasonic-microwave collaborative extraction, ultrasonic power/frequency: 50W/28KHz, microwave power: 550W, microwave frequency: 3000MHz, extraction time is 20min, extraction temperature is 70°C;

(5) filter, adopt vacuum filtration to quickly filter pepper powder and other visible objects, the filter membrane aperture is less than 0.15mm, and the filtrate is collected;

(6) Remove the solvent, adopt vacuum low-temperature rotary concentration to remove the solvent, the vacuum degree is controlled at 0.05MPa, and the temperature is controlled at 40°C;

(7) drying, vacuum drying, the vacuum degree is controlled at 0.08MPa, and the temperature is controlled at 50°C to obtain pepper extract;

(8) Collect the pepper oil and pepper extract to obtain 1.6 parts of pepper flavor substances.

Example 2

Raw materials: 10 parts of fresh pepper with spikes, 80 parts of deionized water, 500 parts of 95% edible alcohol.

Preparation:

(1) Preparation of pepper pulp: select the fresh fruit of pepper with ears without damage by diseases and insect pests as raw material, and some of the colors in the fresh fruit turn yellow, get 10 parts of fresh pepper fruit and add 20 parts of deionized water, grind with a refiner, and make it in the slurry No obvious grains or stalks;

(2) Steam distillation: add 60 parts of water to 10 parts of pepper pulp, heat and boil, and then collect the collector and condenser, and keep the joints sealed; after 4 hours of distillation, collect the oily pepper flavor substances, and use anhydrous sodium sulfate to remove Remove moisture to obtain oily substance and water slurry, wherein the pepper flavor substance of the oily substance is sealed and preserved in a brown glass bottle.

(3) Collect the pepper water slurry, remove most of the water by centrifuging at 10° C. for 3 min at 5000 rpm; add 500 parts of 95% edible alcohol to the centrifuged water slurry in step (2);

(4) Ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/30KHz, microwave power: 600W, microwave frequency: 2500MHz, synergistic extraction for 30min;

(5) filter, adopt vacuum filtration to quickly filter pepper powder and other visible objects, the filter membrane aperture is less than 0.15mm, and the filtrate is collected;

(6) Remove the solvent, adopt vacuum low temperature rotary concentration to remove the solvent, the vacuum degree is controlled at 0.05MPa, and the temperature is controlled at 45°C;

(7) drying, vacuum drying, the vacuum degree is controlled at 0.08MPa, and the temperature is controlled at 50°C to obtain pepper extract;

(8) Collect the pepper oil and pepper extract to obtain 1.6 parts of pepper flavor substances.

Comparative example 1

In this comparative example, pepper dried fruit is used to extract pepper flavor substances, and the preparation method is as follows:

(1) Fresh pepper with spikes is dried until the moisture content is less than 12%, to obtain dried pepper, which is pulverized and sieved until the particle size reaches 40 mesh, to obtain pepper powder;

(2) Take 10 parts of pepper powder and distill them with 500 parts of deionized water for 4 hours to collect oily pepper flavor substances, and remove water with anhydrous sodium sulfate to obtain oil and water slurry, wherein the pepper flavor substances of oily substances are used Store in a sealed brown glass bottle.

(3) Collect the pepper water slurry, remove most of the water by centrifuging at 10° C. for 5 min at 4000 rpm; add 350 parts of 95% edible alcohol to the centrifuged water slurry in step (2);

(4) Ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 300W, microwave frequency: 2450MHz, synergistic extraction for 10min.

Other steps are with embodiment 1.

Comparative example 2

Raw materials: 10 parts of fresh pepper with spikes, 60 parts of deionized water, 350 parts of 95% edible alcohol.

The step (4) of its preparation method is different from Example 1, and other conditions are the same;

Wherein, step (4): ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 300W, microwave frequency: 2450MHz, and synergistic extraction for 20 minutes.

Detection and Analysis of Volatile Flavor Substances in Example 3 Pepper Flavor Substances

Carry out GCMS detection and analysis to the pepper flavor substance sample that embodiment 1 and comparative example 1 make, Fig. 1 is the total ion chromatogram of embodiment 1 pepper flavor substance, Fig. 2 is the total ion of the pepper flavor substance that comparative example 1 makes The flow chart and the quantitative analysis results of the samples are shown in Table 1.

The relative content (%) of flavor substances in different pepper samples of table 1

From the results in Figures 1 and 2, it can be seen that the abundance response value of the sample in Figure 1 reaches 8×10 ⁷ , and the abundance response value of the sample in Figure 2 is 1.4×10 ⁷ . At the same time, the number of chromatographic peaks in Figure 1 is much higher than that of The number of chromatographic peaks in Figure 2. Among them, the higher the response value, the larger the peak area, and the larger the relative percentage content of flavor substances; the more the number of chromatographic peaks, the greater the number of flavor compounds. Combining the results of Figures 1-2 and Table 1, it can be seen that the types and contents of volatile flavor substances in the pepper flavor substances prepared in Example 1 of the present invention are significantly better than those in Comparative Example 1.

The impact of different extraction methods of embodiment 4 on the content of non-volatile flavor substances

This example compares the yield of nonvolatile flavor substances in pepper flavor substances obtained by the following extraction methods and the content of total polyphenols and piperine in nonvolatile flavor substances. The results are shown in Table 2, and several The extraction cost of the method, the results are shown in Table 3.

Heat reflux extraction method: 10 parts of pepper samples are packed in a flask, and 100 parts of 95% ethanol by volume are added for extraction, and the solution is kept boiling in a water bath at 85°C. The pump transports the cooling liquid, so that the steam generated by the boiling solution of the cooling liquid is condensed into the flask through the condenser tube, and so on, and the reflux extraction is repeated for 3 hours. Finally, the reflux extraction solution is concentrated by a rotary evaporator and the solvent is recovered. The concentrated solution is finally vacuum-dried. No volatile flavor substances are obtained.

Microwave extraction method: 10 parts of pepper samples are packed in a flask, and 100 parts of 95% ethanol by volume are added for extraction. The microwave power is 300W to keep the temperature of the solution at 80-90°C. , the cooling liquid is transported through the cooling circulation pump, and the steam generated by the boiling solution of the cooling liquid is condensed into the flask through the condenser tube, so repeated, microwave extraction for 0.5h, and the final extracted solution is concentrated by a rotary evaporator and the solvent is recovered, and the concentrated liquid is finally After vacuum drying, non-volatile flavor substances are obtained.

Ultrasonic extraction method: 10 parts of pepper samples are packed in a flask, and 100 parts of 95% ethanol by volume are added for extraction. Ultrasonic extraction is used in a water bath at 30 ° C. The flask is connected to a condenser tube, and the cooling liquid is connected to the condenser tube, which is passed through a cooling circulation pump. Transport the cooling liquid so that the steam generated by the boiling solution of the cooling liquid is condensed into the flask through the condenser tube, and so on, and the ultrasonic extraction is carried out for 0.5h, and the finally extracted solution is concentrated by a rotary evaporator and the solvent is recovered, and the concentrated liquid is finally vacuum-dried to obtain Non-volatile flavor substances.

After testing, the content of non-volatile flavor substances is shown in Table 2.

Table 2 Effects of different extraction methods on the content of non-volatile flavor substances

Table 3 Extraction time and cost comparison results

The above results show that the yield of pepper flavor substances in the extraction method of the present invention is significantly higher than that of the heat reflux extraction method, microwave extraction method, ultrasonic extraction method and the methods of Comparative Examples 1-2, and the content of the obtained non-volatile flavor substances is also significantly higher . At the same time, compared with other methods, the extraction method of the present invention requires less raw materials, lower power consumption and shorter time to obtain 100 g of pepper flavor substances.

The above is only a preferred embodiment of the present invention, it should be pointed out that, for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications can also be made. It should be regarded as the protection scope of the present invention.

Claims (8)

1. a kind of preparation method of pepper flavor substance, which comprises the steps of:

Step 1: taking pepper fresh fruit that water is added to be beaten, pepper slurry is made, is extracted through steam distillation and obtains grease and aqueous slurry；

Step 2: it takes the aqueous slurry of step 1, ethanol water is added and mixes, through Ultrasonic-microwave synergistic extraction, concentration, drying, Obtain paste；

Step 3: paste described in grease described in collection step 1 and step 2 obtains pepper flavor substance.

2. extracting method according to claim 1, which is characterized in that in the Ultrasonic-microwave synergistic extraction, ultrasonic wave Power be 50W, frequency be 25~35KHz；Microwave power is 550~700W, and microwave frequency is 2500~3500MHz, extraction Time is 15~30min, and extraction temperature is 60~80 DEG C.

3. extracting method according to claim 1, which is characterized in that in Ultrasonic-microwave synergistic extraction described in step 2, The power of ultrasonic wave is 50W, frequency 28KHz；Microwave power is 550W, microwave frequency 3000MHz, and extraction time is 20min, extraction temperature are 70 DEG C.

4. preparation method according to claim 1, which is characterized in that the mass ratio of pepper fresh fruit described in step 1 and water For 1:4~10.

5. the preparation method according to claim 4, which is characterized in that the mass ratio of pepper fresh fruit described in step 1 and water For 1:6.

6. preparation method according to claim 1, which is characterized in that the volume of ethyl alcohol in ethanol water described in step 2 Score is 70%~95%.

7. preparation method according to claim 1, which is characterized in that it is 0.1 that concentration described in step 2, which is specially in vacuum degree, 10~70min is concentrated under conditions of being 35~60 DEG C in~0.9MPa, temperature.

8. the pepper flavor substance that the described in any item preparation methods of claim 1~7 are prepared.