CN107699352A - 一种提高罗马春黄菊油香气品质的方法及其应用 - Google Patents
一种提高罗马春黄菊油香气品质的方法及其应用 Download PDFInfo
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Classifications
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
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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
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
本发明的目的是提供一种提高罗马春黄菊油香气品质的方法及其作用,将罗马春黄菊花低温超微粉碎,再加入一定量的酸、氧化剂和酶在水溶液中混合均匀,协同作用下温育发酵一定时间后,水蒸气蒸馏提取挥发油,提高了罗马春黄菊油的提取率和香气品质,具有复合自然丰富的香气,除了菊花特征香气,还带有花香、果甜香、微凉感等天然气息,刺激性降低,香气品质提高;在卷烟配方烟丝、再造烟叶、梗丝中应用,烟香清晰、具有菊花特征香韵、香气丰富纯净、余味干净,克服了菊花特征香气过于强烈、增大刺激、略有杂气、余味略苦的缺陷。
Description
技术领域
本发明涉及烟用添加剂技术领域,具体涉及一种提高罗马春黄菊油香气品质的方法及其应用。
背景技术
随着人们健康意识的提高,烟厂在解决降低卷烟焦油量、而又能保持或满足卷烟吸食可用性方面所面临的困难日益突出。卷烟随着焦油的逐渐降低,具有香气淡弱、欠丰满、烟气干燥、甜润度不够、舒适度较差等缺陷,为了增进和提高卷烟的烟气浓度和香味,为了增进和提高卷烟的烟气浓度和香味,加香加料技术是一条有效途径。目前烟用香料的制造方法主要有两个,从烟草或其它植物中提取天然香料或者采用传统的化工方法合成香料。植物提取天然香料依然存在提取率低、生产成本高、纯度较低、杂质较多等缺陷。
罗马春黄菊(Euryopspectinatus),又名黄金菊,属草本植物,多年生草本花卉,一年生或多年生草本植物,羽状叶有细裂,花黄色,花心黄色,黄金菊夏季开花;全株具香气,叶略带草香及苹果的香气。罗马春黄菊有疏风清热,平肝明目,避暑消烦,清心解毒消除头痛、止吐、促进结疤、利消化、柔软皮肤且能缓解感冒引起的肌肉痛和生理痛,具舒缓效果;令人放松、稳定情绪,也适合用来改善失眠。是天然的镇定剂,松弛、镇定神经效果特佳;对平滑肌有镇定作用,可放松过度紧张的肌肉,使其达到充分的休息,具有稳定情绪、预防失眠的优异效果。利水,治臌胀。
专利“一种烟用春黄菊提取物的制备方法”(申请号:201610896432.4),取春黄菊花水提得到春黄菊提取物A,由固定化乳酸菌小球发酵,醇沉、浓缩得春黄菊提取物,赋予卷烟特色酸香风格;专利“烟用春黄菊浸膏的制备方法”(授权号ZL201410729542.2)将花、茎部和叶混合进行超临界CO2萃取,加入丙二醇,利用分子蒸馏技术再次分离纯化,最后加入蜂蜜,在卷烟中应用有增加烟气甜润感和改善余味的作用;专利“一种烟用春黄菊香料的制备方法及应用”(申请号:201410699209.1)将黄菊干花浸泡并用水蒸馏提取,收集挥发油A;将蒸馏液体和残渣过滤后用乙醇提取并过滤,得到滤渣和滤液,滤液浓缩后得到B,滤渣干燥后得到春黄菊粗多糖粉末,纯化、水解、美拉德反应得到春黄菊香料C。还未见将罗马春黄菊花进行低温超微粉碎、加入酸、氧化剂和酶,预处理提高提取效率,结合纯化技术,共同提高香气品质的报道。
发明内容
本发明的目的是提供一种提高罗马春黄菊油香气品质的方法及其应用,将罗马春黄菊花低温超微粉碎,再加入一定量的酸、氧化剂和酶在水溶液中混合均匀,进行温育发酵一定时间后,水蒸气蒸馏提取挥发油,提高了罗马春黄菊油的提取率和香气品质,具有复合自然丰富的香气,除了菊花特征香气,还带有花香、果甜香、微凉感等天然气息,刺激性降低,香气品质提高;在卷烟配方烟丝、再造烟叶、梗丝中应用,烟香清晰、具有菊花特征香韵、香气丰富纯净、余味干净,克服了菊花特征香气过于强烈、增大刺激、略有杂气、余味略苦的缺陷。
本发明通过以下技术方案实现:
一种提高罗马春黄菊油香气品质的方法,包括如下步骤:
(1)低温超微粉碎:将罗马春黄菊花放入液氮冷冻超微粉碎机中粉碎成超微粉末;
(2)水解发酵:将罗马春黄菊超微粉末和水按质量比1:8~50混合,加入HCL,调节至pH 2.5-4.5,加入占罗马春黄菊超微粉末质量0.01~0.2%的氧化剂,再加入占罗马春黄菊超微粉末质量比0.01~0.1%的复合酶混合均匀,,加入提取罐中,启动搅拌电机,加热至40~60℃,温育发酵2~15h,所述复合酶为酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶的混合;
(3)水蒸气蒸馏:将提取罐温度提升至98±2℃,水蒸气蒸馏3-6h,制备罗马春黄菊发酵挥发油,常温避光保存。
进一步的,所述液氮冷冻超微粉碎的温度为-2~4℃,超微粉末的目数为250~300目。
进一步的,所述的HCL为分析纯。
进一步的,所述氧化剂为Vc、H2O2、Na2O2,为食品级或分析纯,Vc、H2O2、Na2O2的质量比为1:0.5~2:0.5~2;
进一步的,所述复合酶中酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶均为食品级,除了酸性β-葡萄糖苷酶的酶活为100~10000u/g,其他酶的酶活均为1万-20万u/g,各种酶之间的配比按质量比为1:1~2:0.5~1:1~2。
本发明还提供一种上述方法制备的罗马春黄菊油。
本发明还提供一种上述方法制备的罗马春黄菊油在卷烟配方烟丝、再造烟叶、梗丝中的加香应用,添加量为烟丝、再造烟叶、梗丝质量的0.01~1ppm。
本发明的有益效果是:
(1)低温超微粉碎罗马春黄菊花至250~300目,是为了使罗马春黄菊花原料在较低温度下细胞破壁,致香成分提取效率提高的同时,保护其自然香气成分不被高温破坏;
(2)加入HCL,调节至pH 2.5-4.5,是因为在酸性条件下多糖键易断裂,使多糖大分子酸水解,同时加入氧化剂Vc、H2O2和,是因为氧化剂的活性基团能使多糖C-O-C键发生断裂,强酸和氧化剂联合提高罗马春黄菊花中的多糖水解效率,使更多的多糖分解为较小分子的化合物,利于后期的酶水解;
(3)采用复合酶(酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶)水解发酵酸性罗马春黄菊花超微粉末,进一步分解罗马春黄菊花细胞壁物质如纤维素、蛋白质、果胶等,以及多糖大分子物质为葡萄糖、氨基酸等小分子物质,提高致香成分提取效率,同时将风味前体物质水解为香气物质,而酸和氧化剂能协同促进多糖等大分子的水解,使生物酶发酵水解程度更大;低温超微粉碎细胞破壁、酸、氧化剂、复合酶水解的协同联合作用,使罗马春黄菊花致香成分保持更自然,超微粉水溶液中温育的致香物质种类和含量均增加,经水蒸气蒸馏制备的罗马春黄菊花挥发油,具有复合自然丰富的香气,除了菊花特征香气,还带有花香、果甜香、微凉感等天然气息,刺激性降低,香气品质提高;在卷烟配方烟丝、再造烟叶、梗丝中应用,烟香清晰、具有菊花特征香韵、香气丰富纯净自然、余味干净,克服了菊花特征香气过于强烈、增大刺激、略有杂气、余味略苦的缺陷。该方法所用原料来源广泛,绿色环保,工艺条件简单易操作,成本低,具有产业化前景。
具体实施方式
以下结合具体实施例对本发明进行详细地说明。
实施例1
一种提高罗马春黄菊油香气品质的方法:
(1)低温超微粉碎:将罗马春黄菊花放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度为-2℃,超微粉末的粒径250目;
(2)水解发酵:先将罗马春黄菊超微粉末和水按1:12混合,加入HCL,调节至pH2.8,加入占罗马春黄菊花超微粉末质量0.05%的氧化剂Vc、H2O2和Na2O2(质量比为1:0.5:2),再加入占菊花超微粉末质量0.05%的复合酶(酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,质量比为1:1:0.5:1)混合均匀,加入提取罐中,启动搅拌电机,加热至40℃,温育发酵3h;
(3)水蒸气蒸馏:将提取罐温度提升至98±2℃,水蒸气蒸馏3h制备罗马春黄菊发酵挥发油,常温避光保存。
所述的HCL、Vc、H2O2和Na2O2均为分析纯;
所述的酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,均为食品级,酶活分别为10万u/g、10万u/g、10万u/g、和1000u/g;
本发明发酵提取制备的罗马春黄菊油在卷烟配方烟丝中加香应用,添加量为配方烟丝质量的0.01ppm,与烟气协调,烟香清晰,具有花香、果甜香等复合自然气息,香气丰富纯净,余味干净。
实施例2
一种提高罗马春黄菊油香气品质的方法:
(1)低温超微粉碎:将罗马春黄菊花放入液氮冷冻超微粉碎机中粉碎(0℃),粒径280目;
(2)水解发酵:先将罗马春黄菊超微粉末和水按1:25混合,加入HCL,调节至pH3.0,加入占罗马春黄菊超微粉末质量0.02%的氧化剂Vc、H2O2和Na2O2(质量比为1:1:1.5),再加入占菊花超微粉末质量0.1%的复合酶(酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,质量比为1:1.5:0.8:1.2)混合均匀,加入提取罐中,启动搅拌电机,加热至50℃,温育发酵5h;
(3)水蒸气蒸馏:将提取罐温度提升至98±2℃,水蒸气蒸馏4h得到罗马春黄菊发酵挥发油,常温避光保存。
所述的HCL、Vc、H2O2和Na2O2均为分析纯;
所述的复合酶为酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,均为食品级,酶活分别为10万u/g、15万u/g、20万u/g、2000u/g;
本发明发酵提取制备的罗马春黄菊油在再造烟叶中加香应用,添加量为再造烟叶质量的1ppm,与烟气协调,香气丰富自然,具有果香、甜香等复合自然气息,刺激性降低,余味变好。
实施例3
一种提高罗马春黄菊油香气品质的方法:
(1)低温超微粉碎:将罗马春黄菊花放入液氮冷冻超微粉碎机中粉碎(1℃),粒径300目;
(2)水解发酵:先将罗马春黄菊超微粉末和水按质量比1:30混合,加入HCL,调节至pH 4.0,加入占菊花超微粉末质量0.1%的氧化剂Vc、H2O2和Na2O2(质量比为1:1.5:1),再加入占菊花超微粉末质量0.08%的复合酶(酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,质量比为1:2:0.5:1.5)混合均匀,加入提取罐中,启动搅拌电机,加热至55℃,温育发酵8h;
(3)水蒸气蒸馏:将提取罐温度提升至98±2℃,水蒸气蒸馏5h制备罗马春黄菊发酵挥发油,常温避光保存。
所述的HCL、Vc、H2O2和Na2O2均为分析纯;
所述的复合酶为酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶,均为食品级,酶活分别为15万u/g、20万u/g、10万u/g、1万u/g;
本发明发酵提取制备的罗马春黄菊油在梗丝中加香应用,添加量为梗丝质量的0.7ppm,与烟气协调,香气丰富自然,使杂气减少,余味变好。
试验例1:应用的感官效果评价
将实施例1-3制备的发酵提取的罗马春黄菊油在配方烟丝、再造烟叶及梗丝中进行感官质量评价,样品为施加了本发明春黄菊油的相应配方烟丝、再造烟叶及梗丝,对照组为施加未经前处理直接水蒸气蒸馏春黄菊油和未施加春黄菊油的配方烟丝、再造烟叶及梗丝。
结果表明:本发明方法提高了罗马春黄菊油的提取率和香气品质,除了有菊花的特征香气成分,香气更丰富自然,具有了玫瑰花香、果甜香、微凉感等复合天然气息,香气品质提高;在卷烟配方烟丝、再造烟叶、梗丝中应用,烟香清晰、具有菊花特征香韵、香气丰富纯净、余味干净,克服了菊花特征香气过于强烈、增大刺激、略有杂气、余味略苦的缺陷。
表1.提高香气品质的罗马春黄菊油在配方烟丝中的感官评价
表2.提高香气品质的罗马春黄菊油在再造烟叶中的感官评价
表3.提高香气品质的罗马春黄菊油在梗丝中的感官评价
试验例2:提高香气品质的罗马春黄菊油挥发性成分GC/MS分析
对本发明提高香气品质的罗马春黄菊油与其对照(罗马春黄菊花直接水蒸气蒸馏制备的挥发油)进行挥发性致香成分GC/MS对比分析。
(1)挥发油处理:将挥发油用二氯甲烷萃取、稀释100倍,取1mL用于进行GC/MS分析。
(2)GC/MS分析:HP-5MS(50m×0.25mm×0.25μm)毛细管柱;进样温度:250℃;分流比20:1;载气:He,1mL/min;升温程序:从50℃(1min)以5℃/min升到250℃(5min);传输线温度:250℃;离子源:EI源;电子能量:70eV;扫描范围:50~550amu;使用WILEY和MINILAB谱库进行检索。
(3)挥发性成分对比分析
GC/MS分析结果(表4)表明:
表4发酵提取罗马春黄菊油挥发性成分GC/MS对比分析
由表4可知,罗马春黄菊对照挥发油鉴定出81种挥发性成分,相对百分比含量为72.56%,其中烯25种(41.55%),醇13种,酮8种,醛6种,烷烃6种,酸、酯和酚分别为3种,其他杂环化合物14种;而本发明制备的罗马春黄菊油鉴定出139种挥发性成分,相对百分含量为80.55%,烯37种(34.8651%),醇18种(12.7593%),酮14种,醛12种,烷烃10种,酯7种,酸6种,酚5种,其他杂环化合物30种。
本发明制备的罗马春黄菊油的挥发性成分与对照相比,发生了较大的变化:
(1)新出现的挥发性成分有85种;
(2)挥发性成分相同的有50种,其中相对百分含量增加的有25种,不变的有5种,相对百分含量降低的有20种;
(3)消失的挥发性成分有27种。
很多大分子物质消失或相对百分含量降低,可能是被分解、转化、氧化成了小分子致香物质或香味前体物质。
这些挥发性成分中,单个物质相对百分含量最高的为α-姜黄烯5.25%,其次为2,3,4,5-四甲基-三环[3.2.1.02,7]辛烯4.71%,δ-杜松萜烯3.68%,[1S-(1.α.,5.α.,6.β.)]-双环[3.1.1]庚-2-烯-6-醇、2,7,7-三甲基醋酸酯3.55%,2,5,6-三甲基-1,3,6-庚三烯3.41%,檀香醇3.21%,等。
这些挥发性成分具有自然复合的香气:(+)-α-蒎烯有松木、针叶及树脂样的气息,香气透发,不留长;苯甲醛具有类似苦杏仁的香味;甲基庚烯酮具有柠檬草和乙酸异丁酯般的香气;桉叶油素有樟脑样香气和清凉味道;γ-松油烯具有柑橘和柠檬似香气;芳樟醇是链状萜烯醇类,具有铃兰香气;异环柠檬醛具有香气清鲜有力,柑桔样果香和马鞭草样香韵,较扩散;水芹醛有果子香味;L-薄荷醇具有薄荷香气并有清凉的作用;桃金娘烯醇具有草香、木香和樟脑样香气,气味柔和;薄荷烯酮是一种含氧单萜类成分,具有薄荷气味;β-石竹烯是双环倍半萜类化合物,具有辛香、木香、柑橘香、樟脑香,温和的丁香香气;橙花叔醇具有弱的甜清柔美的橙花气息,带有像玫瑰、铃兰和苹果花的气息;檀香醇具有类似檀香木的香气;马鞭烯醇具特征的马鞭草样香气;(S)-β-红没药烯具有温暖的木香、柑橘香、花香、果香、青香,和甜润的香脂香气;α-荜澄茄油烯具有轻淡的樟木香气;肉豆蔻酸是一种饱和脂肪酸,有柔和烟气的作用;棕榈酸是一种饱和高级脂肪酸,有柔和烟气、协调烟香的作用;植醇具有轻微香气、轻度辛辣味;亚油酸具有类似油脂的香气;等。所有这些糅合在一起,赋予本发明提高香气品质的罗马春黄菊油复合自然丰富的香气,除了菊花特征香气,还带有花香、果甜香、微凉感等天然气息,刺激性降低,香气品质提高。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何属于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。因此,本发明的保护范围应该以权利要求的保护范围为准。
Claims (7)
1.一种提高罗马春黄菊油香气品质的方法,其特征在于包括如下步骤:
(1)低温超微粉碎:将罗马春黄菊花放入液氮冷冻超微粉碎机中粉碎成超微粉末;
(2)水解发酵:将罗马春黄菊超微粉末和水按质量比1:8~50混合,加入HCL,调节至pH2.5-4.5,加入占罗马春黄菊超微粉末质量0.01~0.2%的氧化剂,再加入占罗马春黄菊超微粉末质量比0.01~0.1%的复合酶混合均匀,,加入提取罐中,启动搅拌电机,加热至40~60℃,温育发酵2~15h,所述复合酶为酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶的混合;
(3)水蒸气蒸馏:将提取罐温度提升至98±2℃,水蒸气蒸馏3-6h,制备罗马春黄菊发酵挥发油,常温避光保存。
2.如权利要求1所述的提高罗马春黄菊油香气品质的方法,其特征在于:所述液氮冷冻超微粉碎的温度为-2~4℃,超微粉末的目数为250~300目。
3.如权利要求1所述的提高罗马春黄菊油香气品质的方法,其特征在于:所述的HCL为分析纯。
4.如权利要求1所述的提高罗马春黄菊油香气品质的方法,其特征在于:所述氧化剂为Vc、H2O2、Na2O2的混合,为食品级或分析纯,Vc、H2O2、Na2O2的质量比为1:0.5~2:0.5~2。
5.如权利要求1所述的提高罗马春黄菊油香气品质的方法,其特征在于:所述复合酶中酸性蛋白酶、果聚糖蔗糖酶、酸性纤维素酶、酸性β-葡萄糖苷酶均为食品级,除了酸性β-葡萄糖苷酶的酶活为100~10000u/g,其他酶的酶活均为1万-20万u/g,各种酶之间的配比按质量比为1:1~2:0.5~1:1~2。
6.如权利要求1-5中任一项所述方法制备的罗马春黄菊油。
7.如权利要求1-5中任一项所述方法制备的罗马春黄菊油在卷烟配方烟丝、再造烟叶、梗丝中的加香应用,所述罗马春黄菊油的添加量为烟丝、再造烟叶、梗丝质量的0.01~1ppm。
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