CN106947596B - Preparation method of maltose caramel spice for cigarettes - Google Patents
Preparation method of maltose caramel spice for cigarettes Download PDFInfo
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- CN106947596B CN106947596B CN201710236701.9A CN201710236701A CN106947596B CN 106947596 B CN106947596 B CN 106947596B CN 201710236701 A CN201710236701 A CN 201710236701A CN 106947596 B CN106947596 B CN 106947596B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/305—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation
Abstract
The invention discloses a preparation method of maltose caramel spice for cigarettes, which takes maltose as a raw material, carries out classification separation after reaction in an autoclave, analyzes and researches the quality and style characteristics of cigarettes of all levels of components after separation, and carries out compounding recombination on all levels of separated components on the basis to obtain the maltose caramel spice with different cigarette effects. The maltose caramel adopted by the invention is I-type caramel pigment, so that the safety risk is avoided; and the unique style of the maltose caramel has natural harmony with the cigarette product, and has excellent application effect on enhancing the style characteristics of the cigarette product.
Description
Technical Field
The invention relates to the technical field of cigarette product flavors and fragrances, in particular to a preparation method of a maltose caramel fragrance for cigarettes.
Background
Caramel or caramel pigment is used as a food additive with functions of color matching, flavor blending and seasoning, and is widely applied to the food fields of candies, biscuits, beverages, seasonings and the like. From the current research situation of caramelized pigments, most of caramelized reaction application researches are mainly focused on the color attribute, namely, the research on the aroma attribute is less for obtaining pigment products which have higher color yield, better stability and guaranteed safety and are matched with target color-mixing products. The caramelization reaction is closely related to tobacco, and because the tobacco leaves contain more monosaccharide, disaccharide and oligosaccharide after being prepared, and exogenous sugar serving as a tobacco flavor modifier is also added into tobacco material liquid in a large amount, the caramelization reaction is widely existed in the cigarette processing and burning processes. For example, important aroma components in cigarette smoke, such as 5-methylfurfural, furfural, furfuryl alcohol, furanone, maltol, butanedione and the like, are very typical caramelization reaction products. Theoretically, the caramelization reaction spice has certain innovation and feasibility for supplementing the aroma style of the cigarette product.
However, studies have shown that [ Golon A, Kuhnert N.infraveling the chemical composition of caramels. [ J ]. Journal of Agricultural & Food Chemistry,2012,60(12): 3266-. The caramel pigment contains serial oligosaccharide products with wide molecular weight distribution, serial dehydration products of oligosaccharide, serial hydration products of oligosaccharide, disproportionation reaction products and color flavor high molecular products formed by non-selective glycosylation reaction. Wherein, the components with higher molecular weight are generally considered to have more negative influence on the smoking taste (particularly the mouthfeel) of the cigarette products, and the application of the cigarette caramel in high-grade cigarette products is limited. Moreover, researches indicate that reaction products with different molecular weights also have certain difference on the influence of the internal quality of the cigarettes. Therefore, how to effectively separate and evaluate the caramel according to the molecular weight is the key point for preparing the caramel flavor suitable for cigarettes.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a preparation method of malt sugar caramel spice for cigarettes, and aims to utilize an ultrafiltration technology to carry out fractionation on malt sugar caramel according to molecular weight, systematically evaluate the influence of each stage of isolate on the internal quality of cigarette products, and simultaneously combine sensory evaluation results to carry out compound recombination on the prepared caramel spice so as to obtain the malt sugar caramel spice for cigarettes with different cigarette efficacies and good sensory quality.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the preparation method of the maltose caramel spice of the invention comprises the following steps of firstly, preparing maltose caramel by taking maltose as a sugar source under the conditions of high-pressure nitrogen protection and certain temperature; then, the maltose caramel is subjected to classification separation by adopting spiral flat membrane filtration equipment, and after separation, each grade of separated substance is subjected to sensory evaluation; and finally, recombining and compounding the isolates at all levels according to the sensory evaluation result as required to obtain the maltose caramel essence for the cigarettes. The method comprises the following steps:
(1) dissolving 7.5 parts of maltose powder in 2.5 parts of distilled water at 100 ℃, and placing the solution in an autoclave at 130-150 ℃ and under 3Mpa nitrogen protection for reaction for 2 hours after complete dissolution; after the reaction is finished, cooling and releasing the pressure to normal temperature and normal pressure, taking out the obtained reaction product (maltose caramel), sealing and storing;
(2) adding distilled water with equal mass into the reaction product obtained in the step (1) for dilution, and then performing multi-stage ultrafiltration on the diluted reaction product by adopting spiral flat membrane filtration equipment, wherein the stages of ultrafiltration membranes of each stage are respectively as follows: the first-stage ultrafiltration membrane is 0.22-300 kDa, the second-stage ultrafiltration membrane is 300-100 kDa, the third-stage ultrafiltration membrane is 100-10 kDa, the fourth-stage ultrafiltration membrane is 10-1 kDa, and the fifth-stage ultrafiltration membrane is less than 1 kDa;
respectively adopting distilled water to carry out membrane cleaning on the first-stage retentate to the fourth-stage retentate, and cleaning each stage retentate for 3 times; then combining the three cleaning solutions, concentrating, and freeze-drying to obtain first to fourth-grade samples; directly concentrating the fourth-stage filtrate, and freeze-drying to obtain a fifth-stage sample;
the mass ratio of the volume of the distilled water used in each cleaning to the maltose powder raw material in the step (1) is 8-12 mL: 75 g.
(3) Respectively dissolving the samples of all levels obtained in the step (2) in distilled water to prepare a solution with the mass concentration of 10%, and respectively carrying out injection feeding evaluation on the blank cigarette according to one in a thousand feeding proportion;
(4) and (4) recombining and compounding the products of all levels obtained in the step (2) as required according to the feeding evaluation result of the step (3) to obtain the maltose caramel spice for the cigarettes.
The invention has the beneficial effects that:
firstly, the maltose caramel adopted by the invention is an I-type caramel pigment, ammonia or ammonium catalysts are not added in the preparation of the caramel, harmful components which are easily generated by ammonia/ammonium caramel such as 4-methylimidazole and the like are not generated, and the safety risk is effectively avoided; secondly, the unique caramel of the maltose has the integral style of sweet burnt aroma, sweet honey aroma, sweet baking aroma and fruit aroma and has natural harmony with the cigarette product, and the maltose caramel has excellent application effect on enhancing the style characteristics of the cigarette product; moreover, the maltose caramel is effectively separated through multistage ultrafiltration treatment according to the molecular weight, the proportion of each stage of separated substances is increased or reduced after sensory evaluation, the components of the maltose caramel can be effectively optimized and adjusted, the cigarette effect of the maltose caramel is obviously improved, the composition proportion of each stage of components can be properly adjusted according to actual needs, and different feeding effects are achieved.
Drawings
FIG. 1 is a comparison of the mass percentages of the components of the maltose caramels at two different temperatures in example 1 and example 2.
Detailed Description
The present invention will be described in further detail with reference to examples, which are not intended to limit the scope of the present invention.
Example 1
A preparation method of a maltose caramel spice for cigarettes comprises the following steps:
(1) dissolving 750g of maltose powder in 250g of distilled water at 100 ℃, and placing the solution in an autoclave at 130 ℃ and under 3Mpa for reaction for 2 hours after the maltose powder is completely dissolved; after the reaction is finished, cooling and releasing the pressure to normal temperature and normal pressure, taking out the obtained reaction product, sealing and storing.
(2) Adding distilled water with equal mass into the reaction product obtained in the step (1) for dilution, and then performing multi-stage ultrafiltration on the diluted reaction product by adopting spiral flat membrane filtration equipment, wherein the stages of ultrafiltration membranes of each stage are respectively as follows: 0.22 μm-300kDa (primary), 300kDa-100kDa (secondary), 100kDa-10kDa (tertiary), 10kDa-1kDa (quaternary) and < 1kDa (quinary).
Respectively adopting distilled water to carry out membrane cleaning on the first-stage retentate to the fourth-stage retentate, and cleaning each stage of retentate 3 times with 100mL of distilled water each time; then combining the three cleaning solutions, concentrating, and freeze-drying to obtain first to fourth-grade samples; the fifth sample is directly concentrated from the fourth filtrate and then freeze-dried. The first through fifth samples obtained are labeled A1-A5, respectively.
(3) Dissolving the samples of all levels obtained in the step (2) in distilled water to prepare a solution with the mass concentration of 10%, and performing injection feeding evaluation on the blank cigarette according to one thousandth of feeding proportion.
(4) And (4) recombining and compounding the samples of all levels obtained in the step (2) according to the feeding evaluation result of the step (3) to obtain the maltose caramel spice for the cigarettes.
Example 2
A preparation method of a maltose caramel spice for cigarettes comprises the same steps as example 1, except that the reaction temperature in the step (1) is 150 ℃, and the obtained first to fifth-grade samples are labeled as B1-B5.
The components of example 1 and example 2 were weighed and the mass distribution of the components is shown in FIG. 1. As can be seen from the figure 1, the components with the molecular weight less than 1kDa are the most main components, and the maltose caramels prepared by different processes have obviously different molecular weight distributions and certain mass fractions (one component which can provide enough mass for subsequent compound flavor blending) so as to support the flexibility and the realizability of the compound flavor blending on data.
The separation components of maltose caramel at different temperatures obtained in the above embodiment are prepared into 10% aqueous solution, a blank cigarette is subjected to a feeding experiment according to one in a thousand feeding amount, and smoking evaluation is performed according to YC/T497 + 2014 Chinese style sensory evaluation method (10 cigarettes are provided with cigarette smoking evaluation qualification evaluation committee, and the scores are averaged), and the sensory evaluation results are shown in tables 1 and 2:
TABLE 1 evaluation results of style characteristics of isolates of maltose caramel*
*1Wherein the control is the actual score, and 0 in the score of each separation component indicates no change; "+" indicates reinforcement; "-" indicates weakening
As can be seen from table 1, the main note of the burnt sweet flavor is obviously enhanced along with the increase of the molecular weight of the isolate at 130 ℃, while the notes of spicy flavor, paste flavor, baked flavor, fresh sweet flavor, normal sweet flavor and the like show the trend from enhancement to weakening, wherein the weakening of the baked flavor, the fresh sweet flavor and the normal sweet flavor is extremely obvious; however, overall, the a1-a5 samples had significant effects on enhancing the natural sweet-burnt, baked, milky, fruity, and the like notes.
Under the condition of 150 ℃, the increase of the scorched sweet aroma, the cocoa aroma, the flower aroma and the paste aroma is more obvious along with the increase of the molecular weight of the separated components, and the fragrance notes of spicy aroma, paste aroma, baking aroma, fresh sweet aroma, positive sweet aroma and the like show the tendency of gradual weakening; however, on the whole, B1-B5 has obvious effects on increasing the burnt sweet aroma, the paste aroma, the flower aroma and the cocoa aroma.
Comparing the sensory product absorption data at 130 ℃ and 150 ℃, it can be seen that the separation components at different levels under different temperature conditions have quite different aroma characteristics, such as the style characteristics of scorched sweet, normal sweet, roasted sweet and fruit sweet under 130 ℃; the flavor characteristics of scorched and sweet taste, sweet paste, cocoa fragrance and slight flower fragrance are presented at the temperature of 150 ℃.
TABLE 2 evaluation results of the quality characteristics of the isolates of the maltose caramel grade*
*1Wherein the control is the actual score, and 0 in the score of each separation component indicates no change; "+" indicates improvement; "-" indicates deterioration
From the quality characteristics, as shown in table 2, under the condition of 130 ℃, along with the increase of the molecular weight of the separated components, indexes related to the aroma and the taste of the cigarette, such as oral cavity residual/dry feeling, aroma quality, richness and the like, are rapidly reduced, and smoke indexes, such as fineness, smoke concentration, throat irritation and the like, are improved to a certain extent; the above characteristics are also exhibited as the molecular weight of the separated components increases at 150 ℃.
Comprehensively, the low molecular weight component and the high molecular weight component generally present the following characteristics in the expression of the style and the quality characteristics of the cigarette; (1) the different molecular weight components exhibit distinct characteristics, whether in style or quality characteristics; (2) the low molecular weight component is superior to the high molecular weight component in the expression of aroma indexes, such as richness, aroma texture and the like, and is not superior to the high molecular weight component in the indexes of smoke, such as concentration, softness, fineness and the like.
Therefore, the bright characteristics of various components obtained by treating the maltose caramel by ultrafiltration membranes with different temperatures and different molecular weights provide extremely favorable raw material bases for further compounding and blending the components, and according to the tables 1 and 2, several types of maltose caramel spices for cigarettes are obtained by compounding, and the formula and the function are shown in the table 3.
Table 3 formula and function of compound maltose caramel spice for cigarettes
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (2)
1. A preparation method of a maltose caramel spice for cigarettes is characterized by comprising the following steps: firstly, preparing maltose caramel by taking maltose as a sugar source under the conditions of high-pressure nitrogen protection and certain temperature; then, the maltose caramel is subjected to classification separation by adopting spiral flat membrane filtration equipment, and after separation, each grade of separated substance is subjected to sensory evaluation; finally, according to the sensory evaluation result, recombining and compounding the isolates at all levels as required to obtain the maltose caramel spice for the cigarettes; the method comprises the following steps:
(1) dissolving 7.5 parts of maltose powder in 2.5 parts of distilled water at 100 ℃, and placing the solution in an autoclave at 130-150 ℃ and under 3Mpa nitrogen protection for reaction for 2 hours after complete dissolution; after the reaction is finished, cooling and releasing the pressure to normal temperature and normal pressure, taking out the obtained reaction product, sealing and storing;
(2) adding distilled water with equal mass into the reaction product obtained in the step (1) for dilution, and then performing multi-stage ultrafiltration on the diluted reaction product by adopting spiral flat membrane filtration equipment, wherein the stages of ultrafiltration membranes of each stage are respectively as follows: the first-stage ultrafiltration membrane is 0.22-300 kDa, the second-stage ultrafiltration membrane is 300-100 kDa, the third-stage ultrafiltration membrane is 100-10 kDa, the fourth-stage ultrafiltration membrane is 10-1 kDa, and the fifth-stage ultrafiltration membrane is less than 1 kDa;
respectively adopting distilled water to carry out membrane cleaning on the first-stage retentate to the fourth-stage retentate, and cleaning each stage retentate for 3 times; then combining the three cleaning solutions, concentrating, and freeze-drying to obtain first to fourth-grade samples;
directly concentrating the fourth-stage filtrate, and freeze-drying to obtain a fifth-stage sample;
(3) respectively dissolving the samples of all levels obtained in the step (2) in distilled water to prepare a solution with the mass concentration of 10%, and respectively carrying out injection feeding evaluation on the blank cigarette according to one in a thousand feeding proportion;
(4) and (4) recombining and compounding the samples of all levels obtained in the step (2) as required according to the feeding evaluation result of the step (3) to obtain the maltose caramel spice for the cigarettes.
2. The method of claim 1, wherein: the mass ratio of the volume of the distilled water used in each cleaning in the step (2) to the maltose powder raw material in the step (1) is 8-12 mL: 75 g.
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| CN108720077B (en) * | 2018-07-25 | 2021-04-20 | 河南中烟工业有限责任公司 | Application of low-sugar high-fragrance maple extract in cigarette without burning under heating |
| CN110846133A (en) * | 2019-12-25 | 2020-02-28 | 郑州轻工业大学 | Cigarette caramel spice under negative pressure condition and preparation method thereof |
| CN110839945B (en) * | 2019-12-25 | 2021-07-30 | 郑州轻工业大学 | Preparation method and application of colorless caramel spice |
| CN111254014A (en) * | 2020-03-05 | 2020-06-09 | 四川中烟工业有限责任公司 | Caramel aroma spice, preparation method and application method thereof |
| CN111588073A (en) * | 2020-03-05 | 2020-08-28 | 四川中烟工业有限责任公司 | Burnt sweet-fragrance electronic cigarette tobacco tar, preparation method and application method |
| CN115678680A (en) * | 2022-09-16 | 2023-02-03 | 中国烟草总公司郑州烟草研究院 | Preparation method of characteristic flavor group of natural spice for cigarettes |
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Application publication date: 20170714 Assignee: Anhui jiaotianxiang Biotechnology Co.,Ltd. Assignor: CHINA TOBACCO ANHUI INDUSTRIAL Co.,Ltd. Contract record no.: X2023980036634 Denomination of invention: Preparation method of Maltose caramel flavor for tobacco Granted publication date: 20201225 License type: Exclusive License Record date: 20230620 |