CN118266628A - Method for producing aroma by homogenizing and fermenting cigar tobacco leaves and application - Google Patents
Method for producing aroma by homogenizing and fermenting cigar tobacco leaves and application Download PDFInfo
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- CN118266628A CN118266628A CN202410698112.2A CN202410698112A CN118266628A CN 118266628 A CN118266628 A CN 118266628A CN 202410698112 A CN202410698112 A CN 202410698112A CN 118266628 A CN118266628 A CN 118266628A
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 188
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 188
- 235000019506 cigar Nutrition 0.000 title claims abstract description 83
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims abstract description 37
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001630 malic acid Substances 0.000 claims abstract description 32
- 235000011090 malic acid Nutrition 0.000 claims abstract description 32
- 239000000126 substance Substances 0.000 claims abstract description 25
- XVULBTBTFGYVRC-HHUCQEJWSA-N sclareol Chemical compound CC1(C)CCC[C@]2(C)[C@@H](CC[C@](O)(C)C=C)[C@](C)(O)CC[C@H]21 XVULBTBTFGYVRC-HHUCQEJWSA-N 0.000 claims abstract description 20
- 235000021466 carotenoid Nutrition 0.000 claims abstract description 13
- 150000001747 carotenoids Chemical class 0.000 claims abstract description 13
- 239000012084 conversion product Substances 0.000 claims abstract description 11
- XVULBTBTFGYVRC-UHFFFAOYSA-N Episclareol Natural products CC1(C)CCCC2(C)C(CCC(O)(C)C=C)C(C)(O)CCC21 XVULBTBTFGYVRC-UHFFFAOYSA-N 0.000 claims abstract description 10
- LAEIZWJAQRGPDA-UHFFFAOYSA-N Manoyloxid Natural products CC1(C)CCCC2(C)C3CC=C(C)OC3(C)CCC21 LAEIZWJAQRGPDA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007857 degradation product Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims abstract description 8
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000855 fermentation Methods 0.000 claims description 51
- 230000004151 fermentation Effects 0.000 claims description 51
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 6
- 230000009466 transformation Effects 0.000 claims description 6
- PSQYTAPXSHCGMF-BQYQJAHWSA-N β-ionone Chemical compound CC(=O)\C=C\C1=C(C)CCCC1(C)C PSQYTAPXSHCGMF-BQYQJAHWSA-N 0.000 claims description 6
- SFEOKXHPFMOVRM-UHFFFAOYSA-N (+)-(S)-gamma-ionone Natural products CC(=O)C=CC1C(=C)CCCC1(C)C SFEOKXHPFMOVRM-UHFFFAOYSA-N 0.000 claims description 3
- YKVWPZJHENXDAJ-VOTSOKGWSA-N Megastigmatrienone Chemical compound CC1=CC(=O)CC(C)(C)C1\C=C\C=C YKVWPZJHENXDAJ-VOTSOKGWSA-N 0.000 claims description 3
- POIARNZEYGURDG-FNORWQNLSA-N beta-damascenone Chemical compound C\C=C\C(=O)C1=C(C)C=CCC1(C)C POIARNZEYGURDG-FNORWQNLSA-N 0.000 claims description 3
- 230000003750 conditioning effect Effects 0.000 claims description 3
- CCCXGQLQJHWTLZ-UHFFFAOYSA-N geranyl linalool Natural products CC(=CCCC(=CCCCC(C)(O)CCC=C(C)C)C)C CCCXGQLQJHWTLZ-UHFFFAOYSA-N 0.000 claims description 3
- IQDXAJNQKSIPGB-HQSZAHFGSA-N geranyllinalool Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CCC(C)(O)C=C IQDXAJNQKSIPGB-HQSZAHFGSA-N 0.000 claims description 3
- 229930007850 β-damascenone Natural products 0.000 claims description 3
- LTUMRKDLVGQMJU-UHFFFAOYSA-N famesylacetone Natural products CC(C)=CCCC(C)=CCCC(C)=CCCC(C)=O LTUMRKDLVGQMJU-UHFFFAOYSA-N 0.000 claims description 2
- LTUMRKDLVGQMJU-IUBLYSDUSA-N farnesyl acetone Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CCC(C)=O LTUMRKDLVGQMJU-IUBLYSDUSA-N 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 abstract description 4
- 239000005946 Cypermethrin Substances 0.000 abstract description 2
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 abstract description 2
- 229960005424 cypermethrin Drugs 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract 1
- 238000005070 sampling Methods 0.000 description 28
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 238000004821 distillation Methods 0.000 description 18
- 238000000605 extraction Methods 0.000 description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 230000001143 conditioned effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 210000003462 vein Anatomy 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 239000003283 colorimetric indicator Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 description 1
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 description 1
- 108010005094 Advanced Glycation End Products Proteins 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 239000001729 Ammonium fumarate Substances 0.000 description 1
- 244000233874 Cuphea platycentra Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- NIDGCIPAMWNKOA-WOJBJXKFSA-N Neophytadiene Natural products [C@H](CCC[C@@H](CCCC(C)C)C)(CCCC(C=C)=C)C NIDGCIPAMWNKOA-WOJBJXKFSA-N 0.000 description 1
- 235000002911 Salvia sclarea Nutrition 0.000 description 1
- 244000182022 Salvia sclarea Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940090948 ammonium benzoate Drugs 0.000 description 1
- 235000019297 ammonium fumarate Nutrition 0.000 description 1
- CKKXWJDFFQPBQL-SEPHDYHBSA-N azane;(e)-but-2-enedioic acid Chemical compound N.N.OC(=O)\C=C\C(O)=O CKKXWJDFFQPBQL-SEPHDYHBSA-N 0.000 description 1
- PBLWYVAEJYQTLU-UHFFFAOYSA-N azanium;3-phenylprop-2-enoate Chemical compound [NH4+].[O-]C(=O)C=CC1=CC=CC=C1 PBLWYVAEJYQTLU-UHFFFAOYSA-N 0.000 description 1
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- NIDGCIPAMWNKOA-UHFFFAOYSA-N neophytadiene Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(=C)C=C NIDGCIPAMWNKOA-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- A24B15/20—Biochemical treatment
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/04—Humidifying or drying tobacco bunches or cut tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B9/00—Control of the moisture content of tobacco products, e.g. cigars, cigarettes, pipe tobacco
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
本发明公开一种雪茄烟叶均质化发酵产香的方法及应用,其方法包括以下步骤:S1.将晾制后的雪茄烟叶进行初回潮,并在初回潮后的雪茄烟叶中喷洒pH值为7‑7.5的苹果酸溶液,静置平衡,得到回潮烟叶;S2.将回潮烟叶用纱布包裹,而后发酵,即得产香雪茄烟叶;通过添加苹果酸对雪茄烟叶进行回潮、发酵,不仅提高了发酵后雪茄烟叶的香气含量,同时提高了发酵后烟叶色度、香气含量的均质化度,而且极为显著地提升了类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物、香紫苏醇香气物质的量。The invention discloses a method for producing aroma by homogenizing and fermenting cigar tobacco leaves and an application thereof. The method comprises the following steps: S1. performing initial rehumidification on air-dried cigar tobacco leaves, spraying malic acid solution with a pH value of 7-7.5 on the initially rehumidified cigar tobacco leaves, and allowing the rehumidified tobacco leaves to stand for equilibrium to obtain rehumidified tobacco leaves; S2. wrapping the rehumidified tobacco leaves with gauze, and then fermenting the rehumidified tobacco leaves to obtain aroma-producing cigar tobacco leaves; by adding malic acid to rehumidify and ferment the cigar tobacco leaves, not only the aroma content of the fermented cigar tobacco leaves is increased, but also the homogenization degree of the chromaticity and aroma content of the fermented tobacco leaves is increased, and the amount of carotenoid conversion products, cypermethrin degradation products, phenylalanine conversion products and sclareol aroma substances is significantly increased.
Description
技术领域Technical Field
本发明涉及烟草农业技术领域,尤其涉及一种雪茄烟叶均质化发酵产香的方法及应用。The invention relates to the technical field of tobacco agriculture, and in particular to a method for producing aroma by homogenizing and fermenting cigar tobacco leaves and an application thereof.
背景技术Background technique
雪茄烟叶的发酵制备过程实质上是在一定的温度和湿度条件下,促使烟叶理化特性发生深刻变化,使烟叶糖、氮、碱主要化学成分比例协调、促进内部有机物质降解、分解为香气物质,如类胡萝卜素降解产物、叶绿素降解产物、美拉德反应产物、西柏烷降解产物、苯丙氨酸转化产物等,使烟叶香气和吸味品质明显改善的过程。The fermentation preparation process of cigar tobacco is essentially a process that, under certain temperature and humidity conditions, causes profound changes in the physical and chemical properties of tobacco leaves, coordinates the proportions of the main chemical components of tobacco leaves, such as sugar, nitrogen, and alkali, promotes the degradation of internal organic matter, and decomposes it into aroma substances, such as carotenoid degradation products, chlorophyll degradation products, Maillard reaction products, cedarwood degradation products, phenylalanine conversion products, etc., thereby significantly improving the aroma and smoking quality of tobacco leaves.
雪茄烟叶发酵过程中使用营养剂可以促进烟叶增香。现有营养剂包括草莓酸铵或苯甲酸铵、乙酸铵、酒石酸铵、肉桂酸铵、富马酸铵、异辛酸铵、柠檬酸等等,但是对于雪茄烟叶提高特定香气物质的含量的作用效果不明显,特定香气物质包括类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物、香紫苏醇。The use of nutrients in the fermentation process of cigar tobacco leaves can promote the aroma of tobacco leaves. Existing nutrients include ammonium fragrate or ammonium benzoate, ammonium acetate, ammonium tartrate, ammonium cinnamate, ammonium fumarate, ammonium isooctanoate, citric acid, etc., but the effect of increasing the content of specific aroma substances in cigar tobacco leaves is not obvious, and the specific aroma substances include carotenoid conversion products, ceramsite degradation products, phenylalanine conversion products, and clary alcohol.
因此,有必要提供一种方案以提高雪茄烟叶发酵后特定香气物质含量。Therefore, it is necessary to provide a solution to increase the content of specific aroma substances in cigar tobacco leaves after fermentation.
发明内容Summary of the invention
有鉴于此,本申请提供一种雪茄烟叶均质化发酵产香的方法及应用,用于解决如何提高雪茄烟叶中特定香气物质含量的问题。In view of this, the present application provides a method and application for producing aroma by homogenizing and fermenting cigar tobacco leaves, which is used to solve the problem of how to increase the content of specific aroma substances in cigar tobacco leaves.
为达到上述技术目的,本申请采用以下技术方案:In order to achieve the above technical objectives, this application adopts the following technical solutions:
第一方面,一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:In a first aspect, a method for producing aroma by homogenizing and fermenting cigar tobacco leaves comprises the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮,并在初回潮后的雪茄烟叶中喷洒pH值为7-7.5的苹果酸溶液,静置平衡,得到回潮烟叶;S1. The cigar leaves after airing were initially moistened, and a malic acid solution having a pH value of 7-7.5 was sprayed on the cigar leaves after the initial moistening, and allowed to stand for equilibrium to obtain moistened tobacco leaves;
S2. 将回潮烟叶用纱布包裹,而后发酵,即得产香雪茄烟叶。S2. Wrap the moistened tobacco leaves with gauze and then ferment them to obtain cigar tobacco leaves.
优选的,初回潮后的雪茄烟叶的含水率为20-22%。Preferably, the moisture content of the cigar tobacco leaves after initial moisture conditioning is 20-22%.
优选的,回潮烟叶中的含水率为30-35%。Preferably, the moisture content in the moistened tobacco leaves is 30-35%.
优选的,发酵的条件为:相对湿度75-85%,发酵温度37-39℃,发酵时间为3-14天。Preferably, the fermentation conditions are: relative humidity 75-85%, fermentation temperature 37-39° C., and fermentation time 3-14 days.
优选的,回潮烟叶中,苹果酸的质量浓度为1-5g/kg。Preferably, the mass concentration of malic acid in the tempered tobacco leaves is 1-5 g/kg.
优选的,苹果酸溶液的制备方法为:在苹果酸中加入氨水,调节pH值至7-7.5,即得。Preferably, the preparation method of the malic acid solution is: adding ammonia water to malic acid and adjusting the pH value to 7-7.5.
优选的,纱布的层数为8-10层。Preferably, the number of gauze layers is 8-10 layers.
第二方面,本申请提供一种雪茄烟叶均质化发酵产香的方法提高雪茄烟叶中香气物质含量的应用。In a second aspect, the present application provides a method for producing aroma by homogenizing and fermenting cigar tobacco leaves for use in increasing the content of aroma substances in cigar tobacco leaves.
优选的,香气物质包括类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物、香紫苏醇中的一种或几种。Preferably, the aroma substances include one or more of carotenoid transformation products, ceramsite degradation products, phenylalanine transformation products, and sclareol.
优选的,类胡萝卜素转化产物包括法尼基丙酮、大马酮、巨豆三烯酮、香叶基芳樟醇、β-紫罗酮中的一种或几种。Preferably, the carotenoid conversion product comprises one or more of farnesyl acetone, damascenone, megastigmatrienone, geranyl linalool and β-ionone.
本申请的有益效果如下:The beneficial effects of this application are as follows:
本申请通过添加苹果酸对雪茄烟叶进行回潮、发酵,极为显著提升了类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物、香紫苏醇香气物质的量;The present application adds malic acid to cigar tobacco leaves for moisture conditioning and fermentation, thereby significantly increasing the amount of carotenoid conversion products, cypermethrin degradation products, phenylalanine conversion products, and sclareol aroma substances;
本发明具有补料成分更简单、明确、原料易购、成本低、操作可控性高、适用于雪茄烟叶发酵生产等优点;The invention has the advantages of simpler and clearer feed ingredients, easy purchase of raw materials, low cost, high controllability of operation, and applicability to cigar tobacco leaf fermentation production;
本发明提高了发酵后烟叶色度、香气含量的均质化度,均质化指雪茄烟叶质量的均匀性,雪茄烟叶质量的均匀性包括色度、总香气含量的均匀性。The present invention improves the homogenization degree of the chromaticity and aroma content of the fermented tobacco leaves. The homogenization refers to the uniformity of the quality of the cigar tobacco leaves, and the uniformity of the quality of the cigar tobacco leaves includes the uniformity of the chromaticity and the total aroma content.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
以下通过具体实施例对本方案进行进一步说明。The present solution is further described below through specific embodiments.
原料说明:本申请的实施例及对比例所使用的雪茄烟叶为湖北省恩施雪茄种植基地种植的雪茄植株中部的烟叶,品种为楚雪14。Description of raw materials: The cigar tobacco leaves used in the examples and comparative examples of the present application are tobacco leaves from the middle part of cigar plants grown in the Enshi cigar planting base in Hubei Province, and the variety is Chuxue 14.
实施例1Example 1
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中喷洒用氨水调节后pH值为7的苹果酸溶液,静置平衡,得到回潮烟叶,其中,回潮烟叶苹果酸的质量浓度为1g/kg,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves are initially moistened to a moisture content of 20%, and a malic acid solution having a pH value of 7 adjusted with ammonia water is sprayed on the cigar tobacco leaves after the initial moistening, and the solution is allowed to stand for equilibrium to obtain moistened tobacco leaves, wherein the mass concentration of malic acid in the moistened tobacco leaves is 1 g/kg, and the moisture content of the moistened tobacco leaves is 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%, 37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
实施例2Example 2
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中喷洒用氨水调节后pH值为7的苹果酸溶液,静置平衡,得到回潮烟叶,其中,回潮烟叶苹果酸的质量浓度为2g/kg,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves are initially moistened to a moisture content of 20%, and a malic acid solution having a pH value of 7 adjusted with ammonia water is sprayed on the cigar tobacco leaves after the initial moistening, and the solution is allowed to stand for equilibrium to obtain moistened tobacco leaves, wherein the mass concentration of malic acid in the moistened tobacco leaves is 2 g/kg, and the moisture content of the moistened tobacco leaves is 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%, 37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
实施例3Example 3
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中喷洒用氨水调节后pH值为7的苹果酸溶液,静置平衡,得到回潮烟叶,其中,回潮烟叶苹果酸的质量浓度为3g/kg,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves are initially moistened to a moisture content of 20%, and a malic acid solution having a pH value of 7 adjusted with ammonia water is sprayed on the cigar tobacco leaves after the initial moistening, and the solution is allowed to stand for equilibrium to obtain moistened tobacco leaves, wherein the mass concentration of malic acid in the moistened tobacco leaves is 3 g/kg, and the moisture content of the moistened tobacco leaves is 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%, 37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
实施例4Example 4
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中喷洒用氨水调节后pH值为7的苹果酸溶液,静置平衡,得到回潮烟叶,其中,回潮烟叶苹果酸的质量浓度为4g/kg,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves are initially moistened to a moisture content of 20%, and a malic acid solution having a pH value of 7 adjusted with ammonia water is sprayed on the cigar tobacco leaves after the initial moistening, and the solution is allowed to stand for equilibrium to obtain moistened tobacco leaves, wherein the mass concentration of malic acid in the moistened tobacco leaves is 4 g/kg, and the moisture content of the moistened tobacco leaves is 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%, 37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
实施例5Example 5
一种雪茄烟叶均质化发酵产香的方法,其他内容与实施例1相同,所不同的是回潮烟叶苹果酸的质量浓度为5g/kg。A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, the other contents of which are the same as those of Example 1, except that the mass concentration of malic acid in the conditioned tobacco leaves is 5 g/kg.
实施例6Example 6
一种雪茄烟叶均质化发酵产香的方法:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves:
(1)烟叶回潮(1) Tobacco leaf moisture recovery
将晾制完毕的雪茄烟叶回潮至含水量20~22%后,再称量一定量的水用作回潮水,喷雾喷洒回潮水并翻动烟叶。静置使烟叶中的水分平衡(含水量为34%)。After the air-dried cigar tobacco leaves are re-humidified to a moisture content of 20-22%, a certain amount of water is weighed as re-humidification water, sprayed with the re-humidification water and turned over the tobacco leaves. Let them stand to balance the moisture in the tobacco leaves (moisture content is 34%).
(2)烟叶发酵(2) Tobacco leaf fermentation
雪茄烟叶发酵采用100 kg箱式发酵,发酵房温度30℃、湿度80%。Cigar tobacco leaves are fermented in 100 kg box fermentation rooms with a temperature of 30°C and a humidity of 80%.
箱式发酵烟叶堆垛方式:发酵箱长120 cm,宽80 cm,高80 cm,箱底据地10 cm。烟叶叶柄朝外,层层堆积,在堆好的烟叶上层放上棉布及箱盖。Box-type fermented tobacco stacking method: The fermentation box is 120 cm long, 80 cm wide, 80 cm high, and the bottom of the box is 10 cm from the ground. The tobacco leaves are stacked layer by layer with their petioles facing outwards, and cotton cloth and box cover are placed on the top of the stacked tobacco leaves.
箱式发酵周期:在烟叶堆芯放入温度传感仪,在发酵过程中观察温度变化。当堆温升温至最大值后缓慢降至一定温度,并维持1天左右时翻堆,1个发酵周期8天左右。前期研究确定第3次翻堆雪茄烟叶样品香气含量最高,因而确定第3次翻堆后发酵结束。Box fermentation cycle: Place a temperature sensor in the core of the tobacco pile to observe temperature changes during the fermentation process. When the pile temperature rises to the maximum value and then slowly drops to a certain temperature and maintains for about 1 day, the pile is turned over. One fermentation cycle is about 8 days. Preliminary studies have determined that the aroma content of cigar tobacco samples is the highest after the third turning of the pile, so it is determined that fermentation ends after the third turning of the pile.
发酵过程取样:烟叶发酵前及发酵后(第三次翻堆时)取样。Sampling during the fermentation process: Sampling is taken before and after tobacco fermentation (during the third turning of the pile).
取样方法:将堆垛体按1/3的距离分成上中下三层,每层平面按平面直径1/3处十字交叉为四个取样点,堆芯为一个取样点,共五个取样点,分别随机抽取雪茄烟叶1 Kg。分别为发酵前样品和自然发酵组第3次翻堆样,每个样品为15个取样点(上中下3层,每层5个取样点)所取的烟叶组成。Sampling method: The pile body is divided into three layers at a distance of 1/3, and four sampling points are set at the cross of 1/3 of the plane diameter on each layer. The core is one sampling point, and there are five sampling points in total. 1 kg of cigar tobacco leaves are randomly selected from each of them. They are the samples before fermentation and the third turning samples of the natural fermentation group. Each sample is composed of tobacco leaves taken from 15 sampling points (three layers, top, middle and bottom, 5 sampling points in each layer).
(3)样品色度数值检测(3) Sample chromaticity value detection
利用色差仪对样品进行检测。测定的色度学指标主要包括明度值(L*)、红绿色度值(a*,正值代表红度,负值代表绿度)、黄蓝色度值(b*,正值代表黄度,负值代表蓝度)。从取样点处各抽取3片(上中下3层,每层5个取样点,每个取样点取3片烟叶,共45片)无破损无病斑的代表性叶片作为试验对象进行测量,在每片烟叶叶尖、叶中对称和叶基部对称选取5个点,选点时避开叶脉,进行测量。色度值以上述225个烟叶测定点的测定数据的平均值±标准偏差表示。The samples were tested using a colorimeter. The colorimetric indicators measured mainly include lightness value (L*), red-green value (a*, positive value represents redness, negative value represents greenness), and yellow-blue value (b*, positive value represents yellowness, negative value represents blueness). Three representative leaves without damage or spots were selected from each sampling point (three layers of upper, middle and lower, 5 sampling points in each layer, 3 tobacco leaves were taken from each sampling point, a total of 45 leaves) as test objects for measurement. Five points were selected symmetrically at the tip, middle and base of each tobacco leaf, avoiding the veins when selecting points, and the measurement was performed. The chromaticity value is expressed as the average value ± standard deviation of the measurement data of the above 225 tobacco leaf measurement points.
(4)样品处理及香气物质含量检测(4) Sample processing and aroma substance content detection
每个样品有15个取样点所取的烟叶组成,对这15个取样点的样品分别均匀取样100 g,烘干后用粉碎机粉碎,过40目筛后的样品4℃密封保存。准确称取10 g磨碎后的烟末采用同时蒸馏萃取(SDE)-气质联用(GC-MS)测定烟叶香气物质含量。具体操作如下:取10克烟沫样品置于同时蒸馏萃取装置(SDE)的1000 mL圆底烧瓶中,加入NaCl使其形成饱和食盐水,同时取60 mL二氯甲烷置于另一100 mL圆底烧瓶中,然后将两个圆底烧瓶分别连接在SDE装置两侧;有机相(二氯甲烷)使用55℃水浴加热,水相使用160℃油浴加热,当蒸馏萃取管中有液体回流至两侧烧瓶时开始计时,2 h后收集同时蒸馏萃取后的试液,加入无水硫酸钠除水后,于旋转蒸发仪上减压浓缩至1~2 mL,得到浓缩液。将浓缩液过滤后分别采用气相色谱-质谱联用法(GC-MS)测定香气物质的含量。样品香气物质含量以上述15个取样点样品的测定数据的平均值±标准偏差表示。Each sample consists of tobacco leaves taken from 15 sampling points. 100 g of the samples from these 15 sampling points were evenly sampled, dried and crushed with a pulverizer. The samples after passing through a 40-mesh sieve were sealed and stored at 4°C. 10 g of ground tobacco powder was accurately weighed and the aroma substance content of tobacco leaves was determined by simultaneous distillation extraction (SDE)-gas chromatography-mass spectrometry (GC-MS). The specific operation is as follows: 10 grams of tobacco foam sample was placed in a 1000 mL round-bottom flask of the simultaneous distillation extraction device (SDE), NaCl was added to form saturated salt water, and 60 mL of dichloromethane was placed in another 100 mL round-bottom flask, and then the two round-bottom flasks were connected to both sides of the SDE device; the organic phase (dichloromethane) was heated in a 55°C water bath, and the aqueous phase was heated in a 160°C oil bath. When the liquid in the distillation extraction tube refluxed to the flasks on both sides, the timing was started. After 2 h, the test solution after simultaneous distillation extraction was collected, anhydrous sodium sulfate was added to remove water, and then it was concentrated to 1~2 mL on a rotary evaporator under reduced pressure to obtain a concentrated solution. After filtering the concentrated solution, the content of aroma substances was determined by gas chromatography-mass spectrometry (GC-MS). The content of aroma substances in the sample was expressed as the average value ± standard deviation of the measured data of the samples at the above 15 sampling points.
GC-MS测定条件:色谱柱:HP-5MS毛细管柱(30 m×0.25 mm,0.25 μm);色谱柱升温程序为40℃保持2 min,以2℃/min升至200℃,保持5 min,然后10℃/min升至280℃;载气(He)流速:1 mL/min;进样量:1 μL;分流比:10:1。电子轰击离子源;电子能量70 eV;传输线温度:250℃;离子源温度:230℃;质量扫描范围m/z 35~550。目标化合物的峰识别基于国家标准和技术研究所数据库(NIST14)。烟叶去除主脉烘干后,粉碎过40目筛,使用同时蒸馏萃取装置提取香气成分,使用GC-MS对香气成分进行分析。GC-MS conditions: chromatographic column: HP-5MS capillary column (30 m×0.25 mm, 0.25 μm); the chromatographic column temperature program was 40℃ for 2 min, 2℃/min to 200℃, 5 min, and then 10℃/min to 280℃; carrier gas (He) flow rate: 1 mL/min; injection volume: 1 μL; split ratio: 10:1. Electron bombardment ion source; electron energy 70 eV; transfer line temperature: 250℃; ion source temperature: 230℃; mass scan range m/z 35~550. Peak identification of target compounds was based on the National Institute of Standards and Technology database (NIST14). After the main veins were removed and dried, the tobacco leaves were crushed and passed through a 40-mesh sieve. The aroma components were extracted using a simultaneous distillation extraction device, and the aroma components were analyzed using GC-MS.
中试发酵结束时,实施例6(自然发酵,对照)烟叶亮度值为34±1.9;实施例6(自然发酵,对照))烟叶红绿值为12±0.85;实施例6(自然发酵,对照)烟叶黄蓝值为为18±1.6。At the end of the pilot fermentation, the brightness value of the tobacco leaves of Example 6 (natural fermentation, control) was 34±1.9; the red-green value of the tobacco leaves of Example 6 (natural fermentation, control) was 12±0.85; and the yellow-blue value of the tobacco leaves of Example 6 (natural fermentation, control) was 18±1.6.
样品处理后经同时蒸馏-气质色谱法测定香气物质的含量,发酵前的香气物质的含量为256.84μg/g,实施例6(自然发酵,对照)香气物质的含量为762 μg/g±128.67。After the samples were treated, the content of aroma substances was determined by simultaneous distillation-gas chromatography. The content of aroma substances before fermentation was 256.84 μg/g, and the content of aroma substances in Example 6 (natural fermentation, control) was 762 μg/g±128.67.
实施例7Example 7
一种雪茄烟叶均质化发酵产香的方法:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves:
(1)烟叶回潮(1) Tobacco leaf moisture recovery
将苹果酸溶于温水中,使用氨水调节pH值至7-7.5,制得回潮水。将晾制完毕的雪茄烟叶回潮至含水量20~22%、苹果酸含量为3 g/kg。再称量一定量的水用作回潮水,喷雾喷洒回潮水并翻动烟叶。静置使烟叶中的水分平衡(含水量为34%)。Dissolve malic acid in warm water and use ammonia water to adjust the pH value to 7-7.5 to make rehumidification water. Rehumidify the air-dried cigar tobacco leaves to a moisture content of 20-22% and a malic acid content of 3 g/kg. Weigh a certain amount of water to use as rehumidification water, spray the rehumidification water and turn the tobacco leaves. Let it stand to balance the moisture in the tobacco leaves (moisture content is 34%).
(2)烟叶发酵(2) Tobacco leaf fermentation
雪茄烟叶发酵采用100 kg箱式发酵,发酵房温度30℃、湿度80%。Cigar tobacco leaves are fermented in 100 kg box fermentation rooms with a temperature of 30°C and a humidity of 80%.
箱式发酵烟叶堆垛方式:发酵箱长120 cm,宽80 cm,高80 cm,箱底据地10 cm。烟叶叶柄朝外,层层堆积,在堆好的烟叶上层放上棉布及箱盖。Box-type fermented tobacco stacking method: The fermentation box is 120 cm long, 80 cm wide, 80 cm high, and the bottom of the box is 10 cm from the ground. The tobacco leaves are stacked layer by layer with their petioles facing outwards, and cotton cloth and box cover are placed on the top of the stacked tobacco leaves.
箱式发酵周期:在烟叶堆芯放入温度传感仪,在发酵过程中观察温度变化。当堆温升温至最大值后缓慢降至一定温度,并维持1天左右时翻堆,1个发酵周期8天左右。前期研究确定第3次翻堆雪茄烟叶样品香气含量最高,因而确定第3次翻堆后发酵结束。Box fermentation cycle: Place a temperature sensor in the core of the tobacco pile to observe temperature changes during the fermentation process. When the pile temperature rises to the maximum value and then slowly drops to a certain temperature and maintains for about 1 day, the pile is turned over. One fermentation cycle is about 8 days. Preliminary studies have determined that the aroma content of cigar tobacco samples is the highest after the third turning of the pile, so it is determined that fermentation ends after the third turning of the pile.
发酵过程取样:烟叶发酵前及发酵后(第三次翻堆时)取样。Sampling during the fermentation process: Sampling is taken before and after tobacco fermentation (during the third turning of the pile).
取样方法:将堆垛体按1/3的距离分成上中下三层,每层平面按平面直径1/3处十字交叉为四个取样点,堆芯为一个取样点,共五个取样点,分别随机抽取雪茄烟叶1 Kg。分别为发酵前样品和苹果酸组第3次翻堆样,每个样品为15个取样点(上中下3层,每层5个取样点)所取的烟叶组成。Sampling method: The pile body is divided into three layers at a distance of 1/3, and four sampling points are set at the cross of 1/3 of the plane diameter on each layer. The core is one sampling point, and there are five sampling points in total. 1 kg of cigar tobacco leaves are randomly selected from each of them. They are the samples before fermentation and the third turning samples of the malic acid group. Each sample is composed of tobacco leaves taken from 15 sampling points (three layers, top, middle and bottom, 5 sampling points in each layer).
(3)样品色度数值检测(3) Sample chromaticity value detection
利用色差仪对样品进行检测。测定的色度学指标主要包括明度值(L*)、红绿色度值(a*,正值代表红度,负值代表绿度)、黄蓝色度值(b*,正值代表黄度,负值代表蓝度)。从取样点处各抽取3片(上中下3层,每层5个取样点,每个取样点取3片烟叶,共45片)无破损无病斑的代表性叶片作为试验对象进行测量,在每片烟叶叶尖、叶中对称和叶基部对称选取5个点,选点时避开叶脉,进行测量。色度值以上述225个烟叶测定点的测定数据的平均值±标准偏差表示。The samples were tested using a colorimeter. The colorimetric indicators measured mainly include lightness value (L*), red-green value (a*, positive value represents redness, negative value represents greenness), and yellow-blue value (b*, positive value represents yellowness, negative value represents blueness). Three representative leaves without damage or spots were selected from each sampling point (3 layers, upper, middle and lower, 5 sampling points in each layer, 3 tobacco leaves from each sampling point, a total of 45 leaves) as test objects for measurement. Five points were selected symmetrically at the tip, middle and base of each tobacco leaf, avoiding the veins when selecting points, and the measurement was performed. The chromaticity value is expressed as the average value ± standard deviation of the measurement data of the above 225 tobacco leaf measurement points.
(4)样品处理及香气物质含量检测(4) Sample processing and aroma substance content detection
每个样品有15个取样点所取的烟叶组成,对这15个取样点的样品分别均匀取样100 g,烘干后用粉碎机粉碎,过40目筛后的样品4℃密封保存。准确称取10 g磨碎后的烟末采用同时蒸馏萃取(SDE)-气质联用(GC-MS)测定烟叶香气物质含量。具体操作如下:取10克烟沫样品置于同时蒸馏萃取装置(SDE)的1000 mL圆底烧瓶中,加入NaCl使其形成饱和食盐水,同时取60 mL二氯甲烷置于另一100 mL圆底烧瓶中,然后将两个圆底烧瓶分别连接在SDE装置两侧;有机相(二氯甲烷)使用55℃水浴加热,水相使用160℃油浴加热,当蒸馏萃取管中有液体回流至两侧烧瓶时开始计时,2 h后收集同时蒸馏萃取后的试液,加入无水硫酸钠除水后,于旋转蒸发仪上减压浓缩至1~2 mL,得到浓缩液。将浓缩液过滤后分别采用气相色谱-质谱联用法(GC-MS)测定香气物质的含量。样品香气物质含量以上述15个取样点样品的测定数据的平均值±标准偏差表示。Each sample consists of tobacco leaves taken from 15 sampling points. 100 g of the samples from these 15 sampling points were evenly sampled, dried and crushed with a pulverizer. The samples after passing through a 40-mesh sieve were sealed and stored at 4°C. 10 g of ground tobacco powder was accurately weighed and the aroma substance content of tobacco leaves was determined by simultaneous distillation extraction (SDE)-gas chromatography-mass spectrometry (GC-MS). The specific operation is as follows: 10 grams of tobacco foam sample was placed in a 1000 mL round-bottom flask of the simultaneous distillation extraction device (SDE), NaCl was added to form saturated salt water, and 60 mL of dichloromethane was placed in another 100 mL round-bottom flask, and then the two round-bottom flasks were connected to both sides of the SDE device; the organic phase (dichloromethane) was heated in a 55°C water bath, and the aqueous phase was heated in a 160°C oil bath. When the liquid in the distillation extraction tube refluxed to the flasks on both sides, the timing was started. After 2 h, the test solution after simultaneous distillation extraction was collected, anhydrous sodium sulfate was added to remove water, and then it was concentrated to 1~2 mL on a rotary evaporator under reduced pressure to obtain a concentrated solution. After filtering the concentrated solution, the content of aroma substances was determined by gas chromatography-mass spectrometry (GC-MS). The content of aroma substances in the sample was expressed as the average value ± standard deviation of the measured data of the samples at the above 15 sampling points.
GC-MS测定条件:色谱柱:HP-5MS毛细管柱(30 m×0.25 mm,0.25 μm);色谱柱升温程序为40℃保持2 min,以2℃/min升至200℃,保持5 min,然后10℃/min升至280℃;载气(He)流速:1 mL/min;进样量:1 μL;分流比:10:1。电子轰击离子源;电子能量70 eV;传输线温度:250℃;离子源温度:230℃;质量扫描范围m/z 35~550。目标化合物的峰识别基于国家标准和技术研究所数据库(NIST14)。烟叶去除主脉烘干后,粉碎过40目筛,使用同时蒸馏萃取装置提取香气成分,使用GC-MS对香气成分进行分析。GC-MS conditions: chromatographic column: HP-5MS capillary column (30 m×0.25 mm, 0.25 μm); the chromatographic column temperature program was 40℃ for 2 min, 2℃/min to 200℃, 5 min, and then 10℃/min to 280℃; carrier gas (He) flow rate: 1 mL/min; injection volume: 1 μL; split ratio: 10:1. Electron bombardment ion source; electron energy 70 eV; transfer line temperature: 250℃; ion source temperature: 230℃; mass scan range m/z 35~550. Peak identification of target compounds was based on the National Institute of Standards and Technology database (NIST14). After the main veins were removed and dried, the tobacco leaves were crushed and passed through a 40-mesh sieve. The aroma components were extracted using a simultaneous distillation extraction device, and the aroma components were analyzed using GC-MS.
中试发酵结束时,苹果酸组的烟叶亮度值为36±1.5,而实例6为34±1.9。说明:苹果酸促进了发酵后烟叶的亮度,而且其全箱烟叶的标准偏差降低21%。即:实施例7发酵后烟叶亮度的均匀度提高了21%At the end of the pilot fermentation, the brightness value of the tobacco leaves in the malic acid group was 36±1.5, while that in Example 6 was 34±1.9. This indicates that malic acid promotes the brightness of the tobacco leaves after fermentation, and the standard deviation of the tobacco leaves in the whole box is reduced by 21%. That is, the uniformity of the brightness of the tobacco leaves in Example 7 after fermentation is improved by 21%.
苹果酸组的烟叶红绿值为12±0.81,而实例6(自然发酵,对照)为12±0.85。说明:发酵后烟叶的红色度接近,而且其全箱烟叶的标准偏差降低5%。即:实施例7发酵后烟叶红度的均匀度提高了5%。The red-green value of the tobacco leaves in the malic acid group was 12±0.81, while that of Example 6 (natural fermentation, control) was 12±0.85. Explanation: The redness of the tobacco leaves after fermentation was close, and the standard deviation of the tobacco leaves in the whole box was reduced by 5%. That is, the uniformity of the redness of the tobacco leaves in Example 7 after fermentation was improved by 5%.
苹果酸组的烟叶黄蓝值为20±1.1,而实施例6(自然发酵,对照)为18±1.6。说明:苹果酸促进了发酵后烟叶的黄色度,而且其全箱烟叶的标准偏差降低31%。即:实施例7发酵后烟叶黄色度的均匀度提高了31%。The yellow-blue value of tobacco leaves in the malic acid group was 20±1.1, while that in Example 6 (natural fermentation, control) was 18±1.6. Explanation: Malic acid promoted the yellowness of tobacco leaves after fermentation, and the standard deviation of the whole box of tobacco leaves was reduced by 31%. That is, the uniformity of the yellowness of tobacco leaves in Example 7 after fermentation was improved by 31%.
中试发酵结束时,样品处理后经同时蒸馏-气质色谱法测定香气物质的含量,苹果酸组的香气总量(除新植二烯)为1488 μg/g±52.47,而实施例6(自然发酵,对照)为762 μg/g±128.67。苹果酸促进了发酵后烟叶的香气总量,显著提高了95 %,而且其烟叶总香气含量的标准偏差降低了59%。即:实施例7发酵后烟叶香气总量的均匀度提高了59%。At the end of the pilot fermentation, the sample was treated and the content of aroma substances was measured by simultaneous distillation-gas chromatography. The total aroma of the malic acid group (excluding neophytadiene) was 1488 μg/g±52.47, while that of Example 6 (natural fermentation, control) was 762 μg/g±128.67. Malic acid promoted the total aroma of the fermented tobacco leaves, significantly increasing it by 95%, and the standard deviation of the total aroma content of the tobacco leaves was reduced by 59%. That is, the uniformity of the total aroma of the tobacco leaves after fermentation in Example 7 was increased by 59%.
苹果酸不仅提高了发酵后雪茄烟叶的香气含量,出人意料的是:苹果酸同时提高了色度、香气含量的均质化度,取得了极好的技术效果,为我国雪茄烟叶均质化加工提供了技术方案。Malic acid not only increases the aroma content of fermented cigar tobacco leaves, but surprisingly, it also increases the homogeneity of color and aroma content, achieving excellent technical results and providing a technical solution for the homogenization processing of cigar tobacco leaves in my country.
对比例1Comparative Example 1
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中添加纯水,静置平衡,得到回潮烟叶,其中,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves were initially moistened to a moisture content of 20%, and pure water was added to the cigar tobacco leaves after the initial moistening, and the moistened tobacco leaves were allowed to stand for equilibrium to obtain moistened tobacco leaves, wherein the moisture content of the moistened tobacco leaves was 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%,37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
对比例2Comparative Example 2
一种雪茄烟叶均质化发酵产香的方法,其他内容与实施例2相同,所不同的是,将苹果酸替换为柠檬酸。A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, the other contents of which are the same as those of Example 2, except that malic acid is replaced by citric acid.
对比例3Comparative Example 3
一种雪茄烟叶均质化发酵产香的方法,其他内容与实施例3相同,所不同的是,将苹果酸替换为柠檬酸。A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, the other contents of which are the same as those of Example 3, except that malic acid is replaced by citric acid.
对比例4Comparative Example 4
一种雪茄烟叶均质化发酵产香的方法,其他内容与实施例5相同,所不同的是,将苹果酸替换为柠檬酸。A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, the other contents of which are the same as those of Example 5, except that malic acid is replaced by citric acid.
对比例5Comparative Example 5
一种雪茄烟叶均质化发酵产香的方法,包括以下步骤:A method for producing aroma by homogenizing and fermenting cigar tobacco leaves, comprising the following steps:
S1. 将晾制后的雪茄烟叶进行初回潮至含水量20%,并在初回潮后的雪茄烟叶中称取实施例1中同质量氨水溶解于回潮水中并用稀盐酸调至pH值为7,静置平衡,得到回潮烟叶,其中,回潮烟叶的含水率为34%;S1. The air-dried cigar tobacco leaves are initially conditioned to a moisture content of 20%, and the same mass of ammonia water in Example 1 is weighed and dissolved in the conditioned water, and the pH value is adjusted to 7 with dilute hydrochloric acid, and the conditioned leaves are allowed to stand for equilibrium to obtain conditioned tobacco leaves, wherein the moisture content of the conditioned tobacco leaves is 34%;
S2. 将回潮烟叶用8层纱布包裹并置于不封口的自封袋,每袋自封袋内装有2kg回潮烟叶,而后置于恒温恒湿培养箱中,在相对湿度80%, 37℃,发酵6天,即得产香雪茄烟叶。S2. Wrap the rehydrated tobacco leaves with 8 layers of gauze and place them in unsealed ziplock bags, each containing 2 kg of rehydrated tobacco leaves. Then place them in a constant temperature and humidity incubator at a relative humidity of 80% and 37°C for 6 days to obtain cigar-producing tobacco leaves.
测试与评价Test and Evaluation
对实施例1-4及对比例1得到的产香雪茄烟叶进行处理及香紫苏醇含量检测,方法步骤如下:The cigar tobacco leaves obtained in Examples 1-4 and Comparative Example 1 were processed and the sclareol content was detected, and the steps were as follows:
均匀取样100 g,烘干后用粉碎机粉碎,过40目筛后的样品4℃密封保存。准确称取10 g磨碎后的烟末采用同时蒸馏萃取(SDE)-气质联用(GC-MS)测定烟叶香紫苏醇浓度。具体操作如下:取10 g烟沫样品置于同时蒸馏萃取装置(SDE)的1000 mL圆底烧瓶中,加入NaCl使其形成饱和食盐水,同时取60 mL二氯甲烷置于另一100 mL圆底烧瓶中,然后将两个圆底烧瓶分别连接在SDE装置两侧;有机相(二氯甲烷)使用55℃水浴加热,水相使用160℃油浴加热,当蒸馏萃取管中有液体回流至两侧烧瓶时开始计时,2 h后收集同时蒸馏萃取后的馏出液,加入无水硫酸钠除水后,于旋转蒸发仪上减压浓缩至1~2 mL,得到浓缩液。浓缩液过滤后采用气相色谱-质谱联用法(GC-MS)测定香紫苏醇的含量。100 g of sample was uniformly taken, dried and crushed with a pulverizer, and the sample after passing through a 40-mesh sieve was sealed and stored at 4°C. 10 g of ground tobacco powder was accurately weighed and the concentration of sclareol in tobacco leaves was determined by simultaneous distillation extraction (SDE)-gas chromatography-mass spectrometry (GC-MS). The specific operation was as follows: 10 g of tobacco foam sample was placed in a 1000 mL round-bottom flask of the simultaneous distillation extraction device (SDE), NaCl was added to form saturated salt water, and 60 mL of dichloromethane was placed in another 100 mL round-bottom flask, and then the two round-bottom flasks were connected to both sides of the SDE device; the organic phase (dichloromethane) was heated in a 55°C water bath, and the aqueous phase was heated in a 160°C oil bath. When the liquid in the distillation extraction tube refluxed to the flasks on both sides, the timing was started. After 2 h, the distillate after simultaneous distillation extraction was collected, anhydrous sodium sulfate was added to remove water, and then it was concentrated to 1~2 mL on a rotary evaporator under reduced pressure to obtain a concentrated solution. The concentrated solution was filtered and the content of sclareol was determined by gas chromatography-mass spectrometry (GC-MS).
GC-MS测定条件:色谱柱:HP-5MS毛细管柱(30 m×0.25 mm,0.25 μm);色谱柱升温程序为40℃保持2 min,以2℃/min升至200℃,保持5 min,然后10℃/min升至280℃;载气(He)流速:1 mL/min;进样量:1 μL;分流比:10:1。电子轰击离子源;电子能量70 eV;传输线温度:250℃;离子源温度:230℃;质量扫描范围m/z 35~550。目标化合物的峰识别基于国家标准和技术研究所数据库(NIST14)。GC-MS conditions: chromatographic column: HP-5MS capillary column (30 m×0.25 mm, 0.25 μm); the chromatographic column temperature program was 40°C for 2 min, then increased to 200°C at 2°C/min, maintained for 5 min, and then increased to 280°C at 10°C/min; carrier gas (He) flow rate: 1 mL/min; injection volume: 1 μL; split ratio: 10:1. Electron bombardment ion source; electron energy 70 eV; transfer line temperature: 250°C; ion source temperature: 230°C; mass scan range m/z 35-550. Peak identification of target compounds was based on the National Institute of Standards and Technology database (NIST14).
测试得到实施例1-4及对比例1的样品处理后经同时蒸馏-气质色谱法测定香紫苏醇含量的结果如表1所示。The results of testing the sclareol content of the samples of Examples 1-4 and Comparative Example 1 after treatment by simultaneous distillation-gas chromatography are shown in Table 1.
表1 实施例1-4及对比例1中产香雪茄烟叶香紫苏醇含量测试结果Table 1 Test results of sclareol content in cigar tobacco leaves in Examples 1-4 and Comparative Example 1
对实施例1-5及对比例1-4中产香雪茄烟叶进行处理及类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物含量检测,方法步骤如下:The cigar tobacco leaves produced in Examples 1-5 and Comparative Examples 1-4 were treated and the contents of carotenoid conversion products, ceborane degradation products, and phenylalanine conversion products were detected. The method steps are as follows:
均匀取样100 g,烘干后用粉碎机粉碎,过40目筛后的样品4℃密封保存。准确称取10 g磨碎后的烟末采用同时蒸馏萃取(SDE)-气质联用(GC-MS)测定烟叶香紫苏醇浓度。具体操作如下:取10 g烟沫样品置于同时蒸馏萃取装置(SDE)的1000 mL圆底烧瓶中,加入NaCl使其形成饱和食盐水,同时取60 mL二氯甲烷置于另一100 mL圆底烧瓶中,然后将两个圆底烧瓶分别连接在SDE装置两侧;有机相(二氯甲烷)使用55℃水浴加热,水相使用160℃油浴加热,当蒸馏萃取管中有液体回流至两侧烧瓶时开始计时,2 h后收集同时蒸馏萃取后的馏出液,加入无水硫酸钠除水后,于旋转蒸发仪上减压浓缩至1~2 mL,得到浓缩液。将浓缩液过滤后采用气相色谱-质谱联用法(GC-MS)测定香气含量。100 g of sample was uniformly taken, dried and crushed with a pulverizer, and the sample after passing through a 40-mesh sieve was sealed and stored at 4°C. 10 g of ground tobacco powder was accurately weighed and the concentration of sclareol in tobacco leaves was determined by simultaneous distillation extraction (SDE)-gas chromatography-mass spectrometry (GC-MS). The specific operation was as follows: 10 g of tobacco foam sample was placed in a 1000 mL round-bottom flask of the simultaneous distillation extraction device (SDE), NaCl was added to form saturated salt water, and 60 mL of dichloromethane was placed in another 100 mL round-bottom flask, and then the two round-bottom flasks were connected to both sides of the SDE device; the organic phase (dichloromethane) was heated in a 55°C water bath, and the aqueous phase was heated in a 160°C oil bath. When the liquid in the distillation extraction tube refluxed to the flasks on both sides, the timing was started. After 2 h, the distillate after simultaneous distillation extraction was collected, anhydrous sodium sulfate was added to remove water, and then it was concentrated to 1~2 mL on a rotary evaporator under reduced pressure to obtain a concentrated solution. The concentrate was filtered and the aroma content was determined by gas chromatography-mass spectrometry (GC-MS).
GC-MS测定条件:色谱柱:HP-5MS毛细管柱(30 m×0.25 mm,0.25 μm);色谱柱升温程序为40℃保持2 min,以2℃/min升至200℃,保持5 min,然后10℃/min升至280℃;载气(He)流速:1 mL/min;进样量:1 μL;分流比:10:1。电子轰击离子源;电子能量70 eV;传输线温度:250℃;离子源温度:230℃;质量扫描范围m/z 35~550。目标化合物的峰识别基于国家标准和技术研究所数据库(NIST14)。GC-MS conditions: chromatographic column: HP-5MS capillary column (30 m×0.25 mm, 0.25 μm); the chromatographic column temperature program was 40°C for 2 min, then increased to 200°C at 2°C/min, maintained for 5 min, and then increased to 280°C at 10°C/min; carrier gas (He) flow rate: 1 mL/min; injection volume: 1 μL; split ratio: 10:1. Electron bombardment ion source; electron energy 70 eV; transfer line temperature: 250°C; ion source temperature: 230°C; mass scan range m/z 35-550. Peak identification of target compounds was based on the National Institute of Standards and Technology database (NIST14).
测试结果表2所示。The test results are shown in Table 2.
表2 类胡萝卜素转化产物、西柏烷降解产物、苯丙氨酸转化产物含量检测结果Table 2 Results of the content detection of carotenoid transformation products, ceramidine degradation products, and phenylalanine transformation products
其中,实施例1-4及对比例1得到的产香雪茄烟叶中类胡萝卜素中的含量分布如表3所示,类胡萝卜素包括尼基丙酮、大马酮、巨豆三烯酮、香叶基芳樟醇、β-紫罗酮。The content distribution of carotenoids in the cigar tobacco leaves obtained in Examples 1-4 and Comparative Example 1 is shown in Table 3. Carotenoids include nysyl acetone, damascenone, megastigmatrienone, geranyl linalool, and β-ionone.
表3 类胡萝卜素含量分布Table 3 Distribution of carotenoid content
以上结果说明,本申请使用一定添加量的苹果酸可实现较好的产香增量效果,而使用柠檬酸或者使用苹果酸过量,均不能达到较好的产香增量效果,同时,表2也说明实施例中苹果酸对雪茄烟叶发酵产香的促进作用不是调pH中性后的氨水引起的。The above results indicate that the present application can achieve a better aroma production increment effect by using a certain amount of malic acid, while the use of citric acid or excessive malic acid cannot achieve a better aroma production increment effect. At the same time, Table 2 also indicates that the promoting effect of malic acid on the aroma production of cigar tobacco fermentation in the embodiment is not caused by ammonia water after adjusting the pH to neutral.
以上,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。The above are only preferred specific implementations of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention.
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