Extraction method of vanillin and application of vanillin in tobacco

Abstract

The invention relates to the technical field of vanillin extraction, and provides a vanillin extraction method and application thereof in tobacco, the vanillin extraction method comprises the following steps: S1, taking vanilla pods, crushing, adding a compound enzyme for enzymolysis, and inactivating, filtering and washing to obtain a filtrate; s2, concentrating the filtrate, adding an extracting agent for extraction, centrifuging and filtering to obtain an extracting solution; s3, carrying out extraction, reverse extraction, crystallization, filtration and recrystallization on the extracting solution to obtain vanillin; the extracting agent comprises an organic solvent and water; the organic solvent comprises ethanol and acetonitrile; the volume ratio of the ethanol to the acetonitrile is (1: 9)-(9: 1); the volume ratio of the organic solvent to the water is (1: 1)-(9: 1). According to the technical scheme, the problem that the vanillin extraction yield is low in the prior art is solved.

Description

Technical Field

[0001] The invention relates to the technical field of vanillin extraction, and specifically to a method for extracting vanillin and application thereof on tobacco. Background Art

[0002] Vanillin, chemically known as 3-methoxy-4-hydroxybenzaldehyde, is an important flavor compound widely used in industries such as food, cosmetics, medicine and tobacco. It has a unique vanilla smell, which can add a strong fragrance and flavor to the product and is deeply loved by consumers. In the food industry, vanillin is often used in the seasoning of dairy products, chocolate, cakes, ice cream and other products to improve the taste and quality of the products. In the cosmetics field, vanillin is added to perfumes, skin care products and other products to give them a pleasant aroma. In the pharmaceutical industry, vanillin has certain pharmacological activity and can be used as a drug intermediate or auxiliary ingredient. In the tobacco industry, the application of vanillin is also of great significance. It can improve the aroma of tobacco, improve the quality and taste of tobacco products, and meet consumers' diverse needs for tobacco flavor. At present, one of the sources of vanillin is extracted from vanilla, but the extraction rate of natural vanillin is low and cannot meet market demand. Therefore, how to improve the extraction yield of natural vanillin is a problem that needs to be solved at present. Summary of the invention

[0003] The invention provides a method for extracting vanillin and application thereof on tobacco, thereby solving the problem of low vanillin extraction yield in the related art.

[0004] The technical solution of the present invention is as follows: The present invention provides a method for extracting vanillin, comprising the following steps: S1, taking vanilla pods and crushing them, adding complex enzymes for enzymolysis, inactivating, filtering and washing to obtain a filtrate; S2, concentrating the filtrate, adding an extractant for extraction, and obtaining an extract by centrifugation and filtration; S3, extracting, stripping, crystallizing, filtering and recrystallizing the extract to obtain vanillin; The extractant includes an organic solvent and water; the organic solvent includes ethanol and acetonitrile; the volume ratio of the ethanol to the acetonitrile is 1:9-9:1; the volume ratio of the organic solvent to the water is 1:1-9:1.

[0005] As a further technical solution, the volume ratio of the organic solvent to the water is 4-7:1.

[0006] As a further technical solution, the organic solvent includes ethanol and acetonitrile; the volume ratio of the ethanol to acetonitrile is 3-4:1.

[0007] In the present invention, the extraction yield of vanillin is further improved by limiting the organic solvent in the extractant to include ethanol and acetonitrile, and limiting the volume ratio of ethanol to acetonitrile to 3-4:1.

[0008] As a further technical solution, the complex enzyme includes cellulase and pectinase; the mass ratio of the cellulase to the pectinase is 4:1.

[0009] As a further technical solution, the added amount of the complex enzyme is 0.7% to 1.2% of the mass of the vanilla pods.

[0010] As a further technical solution, the temperature of the enzymolysis is 40-50° C., and the time of the enzymolysis is 3-5 hours.

[0011] As a further technical solution, in step S3, the extract is subjected to pH adjustment, extraction, back extraction, crystallization, filtration, and recrystallization to obtain vanillin; the pH is adjusted to 5-6.

[0012] As a further technical solution, the extraction solvent includes one or more of ethyl acetate, petroleum ether, and n-hexane.

[0013] As a further technical solution, the stripping solvent is a 5 wt % sodium carbonate aqueous solution.

[0014] As a further technical solution, the pH of the crystallization is 4~5, and the temperature of the crystallization is -5~5°C.

[0015] As a further technical solution, the recrystallization solvent includes toluene and n-heptane; the volume ratio of the toluene to the n-heptane is 9-14:1.

[0016] In the present invention, the extraction yield and purity of vanillin are further improved by limiting the recrystallization solvent to include toluene and n-heptane, and limiting the volume ratio of toluene to n-heptane to 9-14:1.

[0017] The invention also provides a method for extracting vanillin and application of the vanillin prepared in tobacco.

[0018] The working principle and beneficial effects of the present invention are: The present invention provides a method for extracting vanillin. Vanillin is extracted by using an extractant composed of acetonitrile, ethanol and water. The obtained vanillin extract is subjected to extraction, back extraction, crystallization, filtration and recrystallization to obtain vanillin. The method improves the yield of naturally extracted vanillin, and the vanillin is applied to tobacco to improve the aroma quality of tobacco. DETAILED DESCRIPTION

[0019] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Example 1 A method for extracting vanillin comprises the following steps: S1. 50 g of vanilla pods were crushed, 100 g of water and 0.35 g of complex enzyme were added, and enzymolysis was performed at 40° C. for 5 h. The filtrate was obtained by inactivation, filtration and washing; S2, concentrating the filtrate, adding 100 mL of an extractant (the volume ratio of ethanol, acetonitrile, and water is 1:9:10) for extraction, and obtaining an extract by centrifugation and filtration; S3, after adjusting the pH of the extract to 5, ethyl acetate was added for extraction, the organic phase was collected, the organic phase was back-extracted with a 5wt% sodium carbonate aqueous solution, the aqueous phase was adjusted to pH 4, crystallized at -5°C, filtered, the filter cake was added to 80mL toluene for recrystallization, filtered again, and dried to obtain 517mg of vanillin with a purity of 94.7% and a yield of 0.98%; The complex enzyme is composed of cellulase and pectinase in a mass ratio of 4:1.

[0021] Example 2 A method for extracting vanillin comprises the following steps: S1. 50 g of vanilla pods were crushed, 100 g of water and 0.6 g of complex enzyme were added, and enzymolysis was performed at 50° C. for 3 h. The filtrate was obtained by inactivation, filtration and washing; S2, concentrating the filtrate, adding 100 mL of an extractant (the volume ratio of ethanol, acetonitrile, and water is 81:9:10) for extraction, and obtaining an extract by centrifugation and filtration; S3, after adjusting the pH of the extract to 6, petroleum ether was added for extraction, the organic phase was collected, and the organic phase was back-extracted with a 5wt% sodium carbonate aqueous solution, the aqueous phase was adjusted to pH 5, and crystallized at 5°C. After filtration, the filter cake was added to 80mL of toluene for recrystallization, filtered again, and dried to obtain 537mg of vanillin with a purity of 94.9% and a yield of 1.02%; The complex enzyme is composed of cellulase and pectinase in a mass ratio of 4:1.

[0022] Example 3 The only difference between this embodiment and embodiment 1 is that the volume ratio of ethanol, acetonitrile and water in the extractant is 8:72:20.

[0023] Results: 599 mg of vanillin was obtained with a purity of 95.1% and a yield of 1.14%.

[0024] Example 4 The only difference between this embodiment and embodiment 1 is that the volume ratio of ethanol, acetonitrile and water in the extractant is 7:63:10.

[0025] Results: 626 mg of vanillin was obtained with a purity of 95.1% and a yield of 1.19%.

[0026] Example 5 The only difference between this embodiment and embodiment 3 is that the volume ratio of ethanol, acetonitrile and water in the extractant is 40:40:20.

[0027] Results: 671 mg of vanillin was obtained with a purity of 95.4% and a yield of 1.28%.

[0028] Example 6 The only difference between this embodiment and embodiment 3 is that the volume ratio of ethanol, acetonitrile and water in the extractant is 60:20:20.

[0029] Result: 707 mg of vanillin was obtained with a purity of 95.5% and a yield of 1.35%.

[0030] Example 7 The only difference between this embodiment and embodiment 3 is that the volume ratio of ethanol, acetonitrile and water in the extractant is 64:16:20.

[0031] Results: 691 mg of vanillin was obtained with a purity of 95.5% and a yield of 1.32%.

[0032] Example 8 The only difference between this embodiment and embodiment 6 is that in step S3, toluene is replaced by equal amounts of toluene and n-heptane in a volume ratio of 4:1.

[0033] Results: 754 mg of vanillin was obtained with a purity of 96.8% and a yield of 1.46%.

[0034] Example 9 The only difference between this embodiment and embodiment 8 is that the volume ratio of toluene to n-heptane is 19:1.

[0035] Results: 764 mg of vanillin was obtained with a purity of 96.9% and a yield of 1.48%.

[0036] Example 10 The only difference between this embodiment and embodiment 8 is that the volume ratio of toluene to n-heptane is 9:1.

[0037] Results: 815 mg of vanillin was obtained with a purity of 97.6% and a yield of 1.59%.

[0038] Embodiment 11 The only difference between this embodiment and embodiment 8 is that the volume ratio of toluene to n-heptane is 14:1.

[0039] Results: 839 mg of vanillin was obtained with a purity of 97.7% and a yield of 1.64%.

[0040] Comparative Example 1 The only difference between this comparative example and Example 1 is that the extractant consists of ethanol and acetonitrile in a volume ratio of 1:9.

[0041] Results: 397 mg of vanillin was obtained with a purity of 93.2% and a yield of 0.74%.

[0042] Comparative Example 2 The only difference between this comparative example and Example 1 is that the extractant consists of ethanol and water in a volume ratio of 1:1.

[0043] Results: 326 mg of vanillin was obtained with a purity of 93.5% and a yield of 0.61%.

[0044] Comparative Example 3 The only difference between this comparative example and Example 1 is that the extractant consists of acetonitrile and water in a volume ratio of 1:1.

[0045] Results: 356 mg of vanillin was obtained with a purity of 94.1% and a yield of 0.67%.

[0046] Compared with Comparative Examples 1 to 3, the extractant in Example 1 consists of ethanol, acetonitrile and water. As a result, the yield of vanillin prepared in Example 1 is higher than that in Comparative Examples 1 to 3, indicating that when the extractant consists of ethanol, acetonitrile and water, the yield of vanillin can be increased.

[0047] Compared with Example 4, Examples 5 to 7 changed the volume ratio of ethanol and acetonitrile in the extractant. As a result, the yield of vanillin obtained in Examples 6 to 7 was higher than that in Examples 4 and 5, indicating that when the volume ratio of ethanol and acetonitrile in the extractant was 3 to 4:1, the yield of vanillin could be further improved.

[0048] Compared with Example 6, Examples 8 to 11 changed the composition of the recrystallization solvent. As a result, the yield and purity of the vanillin obtained in Examples 10 to 11 were higher than those in Examples 6 and 8 to 9, indicating that when the recrystallization solvent consisted of toluene and n-heptane, and the volume ratio of toluene to n-heptane was 9 to 14:1, the purity and yield of vanillin could be improved.

[0049] The vanillin prepared in Example 10 was used as a sample. 5 g of vanillin was weighed and added to 10 g of ethanol (75%) and mixed. Then, 0.01% of the weight of the tobacco was evenly sprayed on 50 g of the tested tobacco with a micro-sprayer. A cigarette without vanillin was used as a blank control group. The tobacco was rolled into cigarettes and placed in a constant temperature and humidity chamber for equilibration for 24 hours. Then, professional smoking evaluation committee members evaluated the cigarettes in accordance with the requirements of GB5606.4-2005 "Cigarettes Part 4: Sensory Technical Requirements". The evaluation standards and evaluation scoring results are shown in Tables 1~2.

[0050] Table 1 Cigarette sensory quality evaluation criteria

[0051] Table 2 Cigarette smoking sensory evaluation scoring results

[0052] Evaluation results: Embodiment 10: The tobacco aroma is full and delicate, without irritation, without impurities, and has good harmony with the tobacco taste.

[0053] Control group: The aroma of the tobacco is light and rough, more irritating, with a slight smell, and is harmonious with the taste of tobacco.

[0054] The results of smoking test show that adding the vanillin prepared in the present invention into shredded tobacco can improve the impurities and irritation in the smoke and enhance the aroma quality of the tobacco.

[0055] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting vanillin, characterized in that: The following steps are involved: S1, taking vanilla pods and crushing them, adding complex enzymes for enzymolysis, inactivating, filtering and washing to obtain a filtrate; S2, concentrating the filtrate, adding an extractant for extraction, and obtaining an extract by centrifugation and filtration; S3, extracting, stripping, crystallizing, filtering and recrystallizing the extract to obtain vanillin; The extractant includes an organic solvent and water; the organic solvent includes ethanol and acetonitrile; the volume ratio of the ethanol to the acetonitrile is 1:9-9:1; the volume ratio of the organic solvent to the water is 1:1-9:

1.

2. The method for extracting vanillin according to claim 1, characterized in that: The volume ratio of the organic solvent to the water is 4-7:

1.

3. The method for extracting vanillin according to claim 1, characterized in that: The volume ratio of the ethanol to acetonitrile is 3-4:

1.

4. The method for extracting vanillin according to claim 1, characterized in that: The complex enzyme comprises cellulase and pectinase; the mass ratio of the cellulase to the pectinase is 4:

1.

5. The method for extracting vanillin according to claim 1, characterized in that: The added amount of the complex enzyme is 0.7% to 1.2% of the mass of the vanilla pods.

6. The method for extracting vanillin according to claim 1, characterized in that: The temperature of the enzymolysis is 40-50° C., and the time of the enzymolysis is 3-5 hours.

7. The method for extracting vanillin according to claim 1, characterized in that: In step S3, the extract is subjected to pH adjustment, extraction, stripping, crystallization, filtration, and recrystallization to obtain vanillin; the pH is adjusted to 5-6.

8. The method for extracting vanillin according to claim 1, characterized in that: The extraction solvent includes one or more of ethyl acetate, petroleum ether and n-hexane.

9. The method for extracting vanillin according to claim 1, characterized in that: The recrystallization solvent includes toluene and n-heptane; the volume ratio of the toluene to the n-heptane is 9-14:

1.

10. Use of the vanillin prepared by the method for extracting vanillin according to any one of claims 1 to 9 in tobacco.

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