Phyllanthus emblica extract as well as preparation method and application thereof

Abstract

The invention provides a phyllanthus emblica extract as well as a preparation method and application thereof. The preparation method comprises the following steps: performing enzymolysis on phyllanthus emblica by using an enzyme preparation to obtain an enzymolysis product; purifying the enzymolysis product by using ethanol to obtain a phyllanthus emblica extract; the enzyme preparation comprises the following effective components: cellulase, hemicellulase, glucosidase, glucose isomerase, pectinase, protease and amylase. According to the method provided by the invention, the cellulose in the phyllanthus emblica is subjected to multi-stage conversion by using the enzyme preparation to finally form a mixture of glucose and fructose, so that the extraction yield of the phyllanthus emblica extract is greatly improved.

Description

Technical Field

[0001] This invention relates to the field of cigarette technology, and in particular to an extract of Phyllanthus emblica, its preparation method, and its application. Background Technology

[0002] Phyllanthus emblica, belonging to the Euphorbiaceae family and the Phyllanthus genus, is a plant whose fresh fruit is sweet, sour, crisp, and slightly astringent, with a sweet aftertaste, hence its name "Yu Gan" (meaning "sweet aftertaste"). It is also known as Hou Gan Zi, An Luo Guo, and Niu Gan Guo. The fruit is spherical or oblate, 1.2-2 cm in diameter. The surface is brownish-brown to dark green, with light yellow granular protrusions, wrinkles, and indistinct six ridges. The fruit stalk is about 1 mm long. Phyllanthus emblica trees are drought-tolerant and can grow in poor soil, exhibiting strong adaptability. They prefer sunlight and warmth. The growing period is 1-3 years. The fruit is sweet, sour, astringent, and cooling. It enters the lung and stomach meridians. It has the effects of clearing heat and cooling the blood, promoting digestion and strengthening the stomach, and promoting body fluid production and relieving cough.

[0003] However, due to the complex composition of Phyllanthus emblica and its high cellulose content, the traditional extraction method yields a low amount of Phyllanthus emblica. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the existing technology and provide a Phyllanthus emblica extract with a high extraction rate, its preparation method, and its application.

[0005] A method for preparing Phyllanthus emblica extract, comprising: S1: Enzymatic hydrolysis of Phyllanthus emblica was performed using an enzyme preparation to obtain the hydrolysis product; S2: The enzymatic hydrolysis product is purified with ethanol to obtain Phyllanthus emblica extract; The active ingredients of the enzyme preparation include: cellulase, hemicellulase, glucosidase, glucose isomerase, pectinase, protease, and amylase.

[0006] Furthermore, in the method for preparing the Phyllanthus emblica extract as described above, the active ingredient of the enzyme preparation, by mass percentage, comprises: Cellulase 1.5~3.0% Hemicellulase 0.5~1.0% Glucosidase 1.0~2.0% Glucose isomerase 0.3~0.8% Pectinase 0.8~1.5% Protease 0.5~0.9% Amylase 0.7~1.2% Ultrapure water: 89.6%~94.7%.

[0007] Further, in the method for preparing the Phyllanthus emblica extract as described above, step S1 includes: S11: Use fresh amla seeds, remove the pits, crush to 50-100 mesh, add 0.5-2.0 times the volume of ultrapure water to make a homogenate, and obtain amla seed homogenate; S12: Enzymatically hydrolyze the amla homogenate using the enzyme preparation to obtain the enzymatic hydrolysis product; enzyme reaction conditions: 45~50℃; pH=5.2~8.0; 48~96 hours.

[0008] Furthermore, the method for preparing Phyllanthus emblica extract as described above, prior to step S12, further includes: The amla homogenate was subjected to ultrasonic pretreatment, and then enzymatic hydrolysis was performed using the ultrasonically pretreated amla homogenate. The ultrasonic pretreatment conditions were: treatment at a constant temperature of 50°C for 1 hour under ultrasonic waves of 200W~2000W.

[0009] Further, in the method for preparing the amla extract as described above, step S2 includes: Add ethanol solution at a ratio of 1:5 for enzymatic hydrolysis product to ethanol, and extract for 2 hours at 35-75℃ with ultrasonic power of 200W-1000W. Filter after extraction. The filtrate was concentrated under reduced pressure at 45°C using a rotary evaporator to a volume of 0.2 to 0.5 times that of the original solution to obtain the amla extract. The ethanol solution has a mass percentage concentration of 95%.

[0010] An extract of Phyllanthus emblica prepared using the method described above.

[0011] The application of the above-mentioned Phyllanthus emblica extract in the cigarette manufacturing process.

[0012] The applications described above include: Preparation of tobacco flavorings using amla extract; The tobacco flavoring is sprayed onto the tobacco shreds.

[0013] As described above, the raw materials for the tobacco flavoring include: Phyllanthus emblica extract, sweet orange oil, rose alcohol, linalyl acetate, amyl butyrate, allyl hexanoate, pear extract, propylene glycol.

[0014] As described above, the raw materials for the tobacco flavoring, by weight percentage, include: The ingredients include 47% Phyllanthus emblica extract, 0.3% sweet orange oil, 0.05% rose alcohol, 0.01% linalyl acetate, 0.01% amyl butyrate, 0.01% allyl hexanoate, 1.6% pear extract, and the balance being propylene glycol.

[0015] The method provided by this invention uses an enzyme preparation to perform multi-stage transformation of cellulose in Phyllanthus emblica, ultimately resulting in a mixture of glucose and fructose, which greatly improves the extraction yield of Phyllanthus emblica extract.

[0016] Water-soluble sugars undergo an acidic reaction during tobacco combustion, which helps regulate the acid-base balance of the smoke. Furthermore, the reactants and derivatives of water-soluble sugars often possess pleasant aromas, harmonizing with the tobacco's aroma and enhancing its concentration. Therefore, cigarettes containing water-soluble sugars have a smoother, more mellow flavor. However, substances like cellulose, pectin, and some polysaccharides can negatively impact the smoke, often producing off-flavors during combustion, increasing irritation, and severely degrading smoke quality. Therefore, this invention utilizes an enzymatic reaction to convert polysaccharides in Phyllanthus emblica into water-soluble monosaccharides, effectively inhibiting their impact on the smoke and also increasing the amount of flavor compounds.

[0017] On the other hand, the cellulose and pectin in Phyllanthus emblica are also major factors affecting the extraction rate. This invention uses enzyme preparations to enzymatically hydrolyze the cellulose, pectin, cell walls and other substances that protect the cytoplasm in Phyllanthus emblica, which can effectively release the volatile aroma components in Phyllanthus emblica cells and achieve full extraction.

[0018] The advantages of enzyme extraction in this invention are: the enzyme's action conditions are very mild and the reaction is simple. Compared with traditional crushing extraction methods, the extraction yield is often not satisfactory due to the coating of high molecular weight compounds such as cellulose and pectin. If extraction is carried out using organic solvents such as petroleum ether and dichloromethane, it will not only pollute the environment but also threaten the health of operators. Enzymatic extraction can not only improve the yield but is also green and environmentally friendly. In addition, the amount of enzyme preparation used is extremely small, which also reduces costs.

[0019] Cellulose Conversion: Phyllanthus emblica has a complex composition and is a fruit rich in cellulose. Traditional extraction methods yield far less cellulose than enzymatic extraction. However, enzymatic extraction suffers from the problem that cellulose forms a gel-like substance after enzymatic hydrolysis, clogging filtration equipment and reducing efficiency. This application utilizes enzymes to perform multi-stage conversion of cellulose, ultimately transforming it into a mixture of glucose and fructose, turning cellulose from waste into a valuable resource and significantly improving upon the shortcomings of traditional extraction methods.

[0020] The advantages of ultrasonic pretreatment in this invention are: before the enzymatic reaction, ultrasonic pretreatment can be used to break down cellulose and cells, thereby effectively releasing the volatile aroma components in the amla cells and achieving full extraction.

[0021] This invention inactivates the enzyme by treating it with ultrasound after enzymatic hydrolysis. The combination of ultrasound and 95% ethanol achieves highly efficient inactivation. Simultaneously, the ultrasound also allows for the more complete release of various active ingredients.

[0022] This invention, through the rational combination of other raw materials, produces a tobacco flavoring with amla extract as the main ingredient, which can improve the quality of cigarettes. Detailed Implementation

[0023] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention are described clearly and completely below. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0024] Example: 1. Pretreatment of Phyllanthus emblica: Use fresh Phyllanthus emblica, remove the pits, crush to 50-100 mesh, and add 0.5-2.0 times the volume of ultrapure water to make Phyllanthus emblica homogenate.

[0025] 2. Ultrasonic pretreatment: The amla syrup was homogenized and treated at a constant temperature of 50°C for 1 hour under an ultrasonic wave of 200W~2000W.

[0026] 3. Enzymatic hydrolysis reaction: Add the prepared enzyme preparation to the amla homogenate at a mass ratio of 1:0.05, adjust the pH to 5.2~8.0, stir at a constant speed at 45~50℃, and the reaction time shall not be less than 48 hours. The proportions of enzyme preparations are as follows: Cellulase 1.5–3.0%, hemicellulase 0.5–1.0%, glucosidase 1.0–2.0%, glucose isomerase 0.3–0.8%, pectinase 0.8–1.5%, protease 0.5–0.9%, amylase 0.7–1.2%, f. ultrapure water 94.7–89.6% Enzyme reaction conditions: 45~50℃; pH 5.2~8.0; 48~96 hours.

[0027] 4. Extraction of reactants: After 48 hours of reaction, add 95% ethanol solution at a ratio of reactants to 95% ethanol of 1:5. Extract for 2 hours at 35-75℃ with ultrasonic power of 200W-1000W. Filter after extraction. Concentrate the filtrate under reduced pressure using a rotary evaporator at 45℃ to 0.2-0.5 times the volume of the original solution to obtain the Phyllanthus emblica extract.

[0028] 5. Blending of tobacco flavorings based primarily on amla extract: Tobacco flavoring formula: Amla extract 47-52%, sweet orange oil (excluding terpenes) 0.3-0.5%, rose alcohol 0.05-0.1%, linalyl acetate 0.01-0.05%, amyl butyrate 0.01-0.025%, allyl hexanoate 0.01-0.03%, pear extract 1.6-2.5%, propylene glycol balance.

[0029] 6. Sensory evaluation experiment: By adding additives to blank tobacco, 10 experienced sensory evaluators smoked flavorings made with amla extract extracted using traditional methods, flavorings made with amla extract extracted using the method of this application, and a blank control group, and gave sensory evaluation scores.

[0030] Example 1 1. Enzyme ratio: Cellulase 1.5%, Pectinase 0.8%, Ultrapure water 97.7% 2. Reaction conditions: 45℃, 5.2 pH, 48h 3. Extraction conditions: 65℃, 200W, 2h 4. Phyllanthus emblica flavoring formula: Phyllanthus emblica extract 47%, sweet orange oil (excluding terpenes) 0.3%, rose alcohol 0.05%, linalyl acetate 0.01%, amyl butyrate 0.01%, allyl hexanoate 0.01%, pear extract 1.6%, propylene glycol 51.02%. 5. Adding ingredients: Spray 0.1% of the ingredients evenly onto 50g of tobacco, then smoke and test the tobacco.

[0031] 6. The results are shown in Table 1: Table 1 As can be seen from Table 1, the enzyme preparation did not react completely with the substrate, resulting in the formation of gel-like substances such as hemicellulose and dextrin, which greatly affected filtration, significantly reduced extraction efficiency, and led to low extraction yield. In addition, the presence of polysaccharides meant that they could not be absorbed by the tobacco shreds during feeding, thus affecting the quality of the tobacco shreds.

[0032] Example 2 1. Enzyme ratio: Cellulase 1.5%, Hemicellulase 0.5%, Glucosidase 1.0%, Glucose isomerase 0.3%, Pectinase 0.8%, Ultrapure water 95.9% 2. Reaction conditions: 45℃, 5.2 pH, 48h 3. Extraction conditions: 65℃, 200W, 2h 4. Phyllanthus emblica flavoring formula: Phyllanthus emblica extract 47%, sweet orange oil (excluding terpenes) 0.3%, rose alcohol 0.05%, linalyl acetate 0.01%, amyl butyrate 0.01%, allyl hexanoate 0.01%, pear extract 1.6%, propylene glycol 51.02%. 5. Adding: Spray 0.1% of the additive evenly onto 10g of tobacco shreds, and then analyze the smoke.

[0033] 6. The results are shown in Table 2: Table 2 As can be seen from Table 2, after adding the corresponding enzymes, most of the polysaccharides can be converted into monosaccharides. Adding this extract to tobacco as an additive can significantly improve the quality of tobacco and smoking quality, reduce the formation of gelatinous substances, and improve extraction efficiency.

[0034] Example 3 1. Enzyme ratio: Cellulase 1.5%, Hemicellulase 0.5%, Glucosidase 1.0%, Glucose isomerase 0.3%, Pectinase 0.8%, Ultrapure water 95.9% 2. Reaction conditions: 50℃, 5.2 pH, 48h 3. Extraction conditions: 75℃, 200W, 2h 4. Phyllanthus emblica flavoring formula: Phyllanthus emblica extract 47%, sweet orange oil (excluding terpenes) 0.3%, rose alcohol 0.05%, linalyl acetate 0.01%, amyl butyrate 0.01%, allyl hexanoate 0.01%, pear extract 1.6%, propylene glycol 51.02%. 5. Adding: Spray 0.1% of the additive evenly onto 10g of tobacco shreds, and then analyze the smoke.

[0035] 6. The results are shown in Table 3: Table 3 As can be seen from Table 3, increasing the temperature correspondingly increases the enzyme activity and improves the yield by 1-2%. Under these conditions, the obtained Phyllanthus emblica extract has a higher content of volatile components and an increased sugar content.

[0036] Example 4 1. Enzyme composition: Cellulase 1.5%, Hemicellulase 0.5%, Glucosidase 1.0%, Glucose Isomerase 0.8%, Pectinase 0.8%, Amylase 0.9%, Protease 0.7%, Ultrapure Water 93.8% 2. Reaction conditions: 50℃, 7.3pH, 96h 3. Extraction conditions: 75℃, 200W, 2h 4. Phyllanthus emblica flavoring formula: Phyllanthus emblica extract 47%, sweet orange oil (excluding terpenes) 0.3%, rose alcohol 0.05%, linalyl acetate 0.01%, amyl butyrate 0.01%, allyl hexanoate 0.01%, pear extract 1.6%, propylene glycol 51.02%. 5. Adding ingredients: Spray 0.1% of the ingredients evenly onto 10g of tobacco, then smoke and test the tobacco.

[0037] 6. The results are shown in Table 4: Table 4 As can be seen from Table 4, by increasing the amount of glucose isomerase, the ratio of glucose and fructose in the extract became more balanced. Furthermore, by increasing the reaction temperature, extraction temperature, and reaction time, the reaction became more complete, most of the substrate was consumed, and more active ingredients were released, resulting in a 2-3% increase in the yield of active ingredients in the extract.

[0038] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing an extract of Phyllanthus emblica, characterized in that, include: S1: Enzymatic hydrolysis of Phyllanthus emblica was performed using an enzyme preparation to obtain the hydrolysis product; S2: The enzymatic hydrolysis product is purified with ethanol to obtain Phyllanthus emblica extract; The active ingredients of the enzyme preparation include: cellulase, hemicellulase, glucosidase, glucose isomerase, pectinase, protease, and amylase.

2. The method for preparing Phyllanthus emblica extract according to claim 1, characterized in that, The active ingredients of the enzyme preparation, by mass percentage, include: Cellulase 1.5~3.0% Hemicellulase 0.5~1.0% Glucosidase 1.0~2.0% Glucose isomerase 0.3~0.8% Pectinase 0.8~1.5% Protease 0.5~0.9% Amylase 0.7~1.2% Ultrapure water: 89.6%~94.7%.

3. The method for preparing Phyllanthus emblica extract according to claim 1 or 2, characterized in that, S1 includes: S11: Use fresh amla seeds, remove the pits, crush to 50-100 mesh, add 0.5-2.0 times the volume of ultrapure water to make a homogenate, and obtain amla seed homogenate; S12: Enzymatically hydrolyze the amla homogenate using the enzyme preparation to obtain the enzymatic hydrolysis product; enzyme reaction conditions: 45~50℃; pH=5.2~8.0; 48~96 hours.

4. The method for preparing Phyllanthus emblica extract according to claim 3, characterized in that, Before step S12, the following is also included: The amla homogenate was subjected to ultrasonic pretreatment, and then enzymatic hydrolysis was performed using the ultrasonically pretreated amla homogenate. The ultrasonic pretreatment conditions were: treatment at a constant temperature of 50°C for 1 hour under ultrasonic waves of 200W~2000W.

5. The method for preparing Phyllanthus emblica extract according to claim 1, characterized in that, S2 includes: Add ethanol solution at a ratio of 1:5 for enzymatic hydrolysis product to ethanol, and extract for 2 hours at 35~75℃ with ultrasonic power of 200W-1000W. Filter after extraction. The filtrate was concentrated under reduced pressure at 45°C using a rotary evaporator to a volume of 0.2 to 0.5 times that of the original solution to obtain the amla extract. The ethanol solution has a mass percentage concentration of 95%.

6. An extract of Phyllanthus emblica prepared by any one of the methods described in claims 1-5.

7. The use of the amla extract according to claim 6 in the preparation of cigarettes.

8. The application according to claim 7, characterized in that: include: Preparation of tobacco flavorings using amla extract; The tobacco flavoring is sprayed onto the tobacco shreds.

9. The application according to claim 8, characterized in that: The raw materials for the tobacco flavoring include: Phyllanthus emblica extract, sweet orange oil, rose alcohol, linalyl acetate, amyl butyrate, allyl hexanoate, pear extract, propylene glycol.

10. The application according to claim 9, characterized in that: The raw materials for the tobacco flavoring, by weight percentage, include: Phyllanthus emblica extract 47%, sweet orange oil 0.3%, rose alcohol 0.05%, linalyl acetate 0.01%, amyl butyrate 0.01%, allyl hexanoate 0.01%, pear extract 1.6%, propylene glycol balance.

Images