阅读说明：本技术 一种烟用黑枸杞香料的制备方法及在卷烟中的应用 (Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes ) 是由 吴彦 薛云 胡志忠 刘启斌 宋凌勇 农李政 李志华 刘鸿 陈义昌 宁振兴 白家峰 于 2020-07-20 设计创作，主要内容包括：本发明提供了一种烟用黑枸杞香料的制备方法：黑枸杞粉碎过筛,加质量比3％蔗糖,然后乙醇为溶剂,索氏提取法提取和超声波提取、过滤,浓缩得到黑枸杞浸膏；黑枸杞浸膏乙醇溶解,使用陶瓷膜过滤除去大分子物质；陶瓷膜透过液有机膜过滤,去除滤过部分影响香气与口感的小分子物质,有机膜截留部分减压蒸馏浓缩,得到黑枸杞香料。本发明还提供了该香料在卷烟中的应用：将烟用黑枸杞香料进行稀释,以一定比例喷洒于烟丝卷制成卷烟。添加该香料后,能明显降低刺激性和杂气,甜润感增加,余味舒适。(The invention provides a preparation method of a lycium ruthenicum spice for cigarettes, which comprises the following steps: crushing and sieving the lycium ruthenicum, adding sucrose with the mass ratio of 3%, then taking ethanol as a solvent, extracting by a Soxhlet extraction method, performing ultrasonic extraction, filtering, and concentrating to obtain a lycium ruthenicum extract; dissolving the Lycium ruthenicum Murr extract with ethanol, and filtering with ceramic membrane to remove macromolecular substances; filtering the ceramic membrane permeate by an organic membrane to remove small molecular substances affecting the fragrance and the taste of the filtered part, and distilling and concentrating the intercepted part of the organic membrane under reduced pressure to obtain the Lycium ruthenicum Murr spice. The invention also provides the application of the spice in cigarettes: diluting fructus Lycii spice for cigarette, and spraying onto tobacco shred to make cigarette. After the perfume is added, the irritation and miscellaneous gas can be obviously reduced, the sweet feeling is increased, and the aftertaste is comfortable.)

1. The preparation method of the lycium ruthenicum for the cigarettes is characterized by comprising the following steps of:

(1) crushing: pulverizing dried fructus Lycii into coarse powder, and sieving with 60-80 mesh stainless steel screen;

(2) soxhlet extraction: weighing a certain amount of lycium ruthenicum raw material, placing the raw material into a Soxhlet extractor, adding sucrose with the mass ratio of 2-5%, adding 50% -100% ethanol with the mass ratio of 5-10 times, heating to 50-100 ℃, and heating and refluxing for 1-3 h; centrifuging to obtain filtrate A and filter residue;

(3) ultrasonic extraction: carrying out ultrasonic extraction on the filter residue obtained in the step (2), adding 4-8 times of 40% -80% ethanol water solution, and carrying out ultrasonic treatment at 50-70 ℃ for 30-70 min and 50-60 kHz ultrasonic frequency; centrifuging to obtain filtrate B, and mixing the filtrate A and the filtrate B to obtain Lycium ruthenicum Murr extract;

(4) alcohol collection and concentration: carrying out reduced pressure distillation and concentration on the mixed extracting solution in the step (3) in a rotary evaporator to obtain an extractum, and obtaining a lycium ruthenicum extract;

(5) and (3) separating with a microfiltration membrane: accurately weighing Lycium ruthenicum Murr extract, adding 40-50 times of 20-50% ethanol, and dissolving to obtain H1 solution; after complete dissolution, filtering with 50-200nm ceramic microfiltration membrane, wherein the interception section is H2;

(6) and (3) ultrafiltration membrane separation: filtering the microfiltration membrane permeate by using an organic membrane with the concentration of 10-500kd, wherein the interception section is marked as H3, and the permeation section is marked as H4;

(7) and (3) reduced pressure distillation: distilling H3 part under reduced pressure to relative density of 1.05-1.15 to obtain Lycium ruthenicum Murr essence.

2. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein 5-8 times of 70-95% ethanol is added in the step (2), the heating temperature is 65-85 ℃, and the heating reflux is carried out for 1-3 hours; filtering to obtain filtrate A and filter residue.

3. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (2), the mass ratio of the added cane sugar is 3%; adding 85-90% ethanol in an amount which is 5-6 times that of the raw materials, heating to 75-80 ℃, and heating and refluxing for 1-3 h; filtering to obtain filtrate A and filter residue.

4. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (3), 50% -70% of ethanol aqueous solution which is 5-7 times of the amount of the lycium ruthenicum spice is added, the ultrasonic temperature is 60-70 ℃, the ultrasonic time is 40-60min, and the ultrasonic frequency is 50kHz-60 kHz.

5. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (3), 55% -60% of ethanol aqueous solution which is 5-6 times of the amount of the lycium ruthenicum spice is added, the ultrasonic temperature is 60-65 ℃, the ultrasonic time is 45-50min, and the ultrasonic frequency is 50kHz-60 kHz.

6. The preparation method of lycium ruthenicum mill flavor for cigarettes according to claim 1, wherein in the step (5), the pore diameter of the microfiltration membrane is 50-100 nm.

7. The preparation method of lycium ruthenicum murr spice for cigarettes according to claim 1, wherein in the step (6), the pore size of the ultrafiltration membrane is 50-200 KD.

8. The preparation method of lycium ruthenicum murr spice for cigarettes according to claim 1, wherein in the step (6), the pore size of the ultrafiltration membrane is 50-100 KD.

9. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 10-100; before preparing cigarettes, the lycium ruthenicum spice for cigarettes is sprayed on tobacco shreds according to the mass ratio of 0.02-1%, and then the cigarettes are prepared.

10. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 20-70; before preparing cigarettes, spraying the lycium ruthenicum spice for cigarettes on tobacco shreds according to the mass ratio of 0.05-0.5%, and rolling into cigarettes.

11. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 40-50; before preparing cigarettes, spraying the lycium ruthenicum spice for cigarettes on tobacco shreds according to the mass ratio of 0.1-0.3%, and rolling into cigarettes; the organic solvent is ethanol, propylene glycol, sorbitol, xylitol or glycerol, or a mixed solution of more than 2 of the above.

Technical Field

The invention belongs to the technical field of preparation of cigarette additives, and particularly relates to a preparation method of a lycium ruthenicum spice for cigarettes and application of the lycium ruthenicum spice in cigarettes.

Background

Lycium ruthenicum Murr is a special wild plant in northwest China, and mature fruits of the Lycium ruthenicum Murr are rich in anthocyanin, lycium barbarum polysaccharide, amino acid, vitamin and trace elements. Loshuting et al measure the volatile components in Lycium ruthenicum Murr by SPME-GC/MS method. The results show that the volatile components in Lycium ruthenicum Murr contain fragrance substances such as limonene, caryophyllene, citral, beta-ionone, ethyl laurate, farnesyl acetaldehyde and the like, and many of the volatile components are important components of natural perfume. The application of Lycium ruthenicum Murr products in cigarettes is rarely reported.

The natural fragrant components extracted by the conventional extraction method, such as the Soxhlet extraction method and the like, inevitably contain impurities, such as protein, starch, wax and the like, which not only affect the quality of natural spices, but also affect the perfuming effect of cigarettes, and simultaneously have certain influence on the smoking safety of the cigarettes.

Membrane separation technology refers to a technology in which a mixture of molecules of different particle sizes on a molecular level is selectively separated while passing through a semipermeable membrane. The membrane separation technology can effectively remove macromolecular substances which have negative influence on the sensory quality of smoke while keeping the original characteristic fragrance of the extract, thereby achieving the purpose of improving the quality of the extract. However, the preparation of the tobacco flavor by separating the lycium ruthenicum extract by using a membrane separation technology is not seen.

The prepared lycium ruthenicum extract is separated and purified by a membrane separation technology, so that impurities such as protein, starch, wax and the like in the extract can be removed, meanwhile, small molecular substances influencing the fragrance can be removed by ultrafiltration or nanofiltration membrane separation and interception, and refined natural perfume components are obtained.

Disclosure of Invention

The invention aims to provide a preparation method of lycium ruthenicum murr spice for cigarettes, which has an obvious aroma enhancement effect and few impurities, aiming at the defects of the existing preparation method of the spice for cigarettes, particularly the lycium ruthenicum murr spice for cigarettes. The invention is realized by the following technical scheme:

in order to achieve the aim, the preparation method of the lycium ruthenicum spice for the cigarettes comprises the following steps: (1) crushing: pulverizing dried fructus Lycii into coarse powder, and sieving with 60-80 mesh stainless steel screen;

(2) soxhlet extraction: accurately weighing Lycium ruthenicum Murr powder, placing in a Soxhlet extractor, adding sucrose 2-5 wt%, adding 50-100% ethanol 5-10 times of the weight of the powder, heating at 50-100 deg.C, and refluxing for 1-3 hr. Filtering to obtain filtrate A and filter residue.

(3) Ultrasonic extraction: and (4) carrying out ultrasonic extraction on the filter residue obtained in the step (3), adding 4-8 times of 40-80% ethanol water solution, and carrying out ultrasonic treatment at 50-70 ℃ for 30-70 min and 50-60 kHz ultrasonic frequency. Centrifuging to obtain filtrate B, and mixing the filtrate A and the filtrate B to obtain the Lycium ruthenicum Murr extract.

(4) Alcohol collection and concentration: and (4) carrying out reduced pressure distillation and concentration on the mixed extracting solution in the step (4) in a rotary evaporator to obtain an extractum, thus obtaining the lycium ruthenicum extract.

(5) And (3) separating with a microfiltration membrane: accurately weighing Lycium ruthenicum Murr extract, placing into a quantitative glass container, adding 40-50 times of 20-50% ethanol, and dissolving to obtain solution H1. After complete dissolution, filtering with 50-200nm ceramic microfiltration membrane, wherein the interception section is H2;

(6) and (3) ultrafiltration membrane separation, namely filtering the microfiltration membrane permeate by using an organic membrane with the concentration of 10-500kd, wherein the interception section is marked as H3, and the permeation section is marked as H4.

(7) Distilling H3 part under reduced pressure to relative density of 1.05-1.15 to obtain Lycium ruthenicum Murr essence.

Further, in the step (2), after sucrose with a mass ratio of preferably 3% is added, the amount of ethanol added is preferably 5 to 8 times, and more preferably 5 to 6 times; the concentration of the ethanol is preferably 70-95%, and more preferably 85-90%; the heating temperature is preferably 65-85 ℃, and more preferably 75-80 ℃;

further, in the step (3), ethanol is added preferably in an amount of 5 to 7 times, and more preferably in an amount of 5 to 6 times; the concentration of the ethanol is preferably 50% -70%, and is further preferably 55% -60%; the ultrasonic temperature is 60-70 ℃, and further preferably 60-65 ℃; the ultrasonic treatment time is preferably 40 to 60min, and more preferably 45 to 50 min.

Further, in the step (5), the pore diameter of the microfiltration membrane is preferably 50-100 nm;

further, in the step (6), the pore size of the ultrafiltration membrane is preferably 50-200KD, and more preferably 50-100 KD;

the lycium ruthenicum murr is one or more of Xinjiang, Qinghai and Gansu.

The invention discloses application of a lycium ruthenicum spice for cigarettes, which comprises the following steps: diluting the lycium ruthenicum spice for the cigarettes by using an organic solvent, wherein the dilution times are 10-100 times; before preparing cigarettes, the lycium ruthenicum spice for cigarettes is sprayed on tobacco shreds according to the mass ratio of 0.02-1%, and then the cigarettes are prepared.

Further, in the application of the lycium ruthenicum spice for the cigarettes, the dilution times of an organic solvent are optimized to be 20-70 times, and further optimized to be 40-50 times; the adding proportion of the tobacco shreds is optimized to be 0.05-0.5 percent, and is further optimized to be 0.1-0.3 percent.

Further, the organic solvent is ethanol, propylene glycol, sorbitol, xylitol or glycerol, or a mixture of any 2 or more thereof.

The application effect of the lycium ruthenicum spice for the cigarettes is characterized in that after the lycium ruthenicum spice is added into the cigarettes, the irritation and the miscellaneous gas can be obviously reduced, the sweet feeling is increased, and the aftertaste is comfortable.

The invention has the advantages that:

compared with the prior art, the membrane separation microfiltration method is utilized to remove a large amount of protein, pectin, starch, wax, cellulose and pigment substances contained in the lycium ruthenicum extract, and the problem of poor sensory comfort caused by burning and sucking the components added into tobacco shreds is avoided. In addition, the invention removes some small molecular substances which influence the aroma quality and the aroma quantity and have irritation in the lycium ruthenicum extract by using a membrane separation ultrafiltration method, reserves proper aroma components in the lycium ruthenicum extract as far as possible, reduces miscellaneous gas and irritation, and removes large molecular and small molecular impurities in the lycium ruthenicum extract, so that the application effect of the lycium ruthenicum extract is better.

The specific implementation mode is as follows: