CN105733811A - 一种葡萄糖苷酶促生香制备灵香草挥发油的方法及其应用 - Google Patents
一种葡萄糖苷酶促生香制备灵香草挥发油的方法及其应用 Download PDFInfo
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- CN105733811A CN105733811A CN201610093601.0A CN201610093601A CN105733811A CN 105733811 A CN105733811 A CN 105733811A CN 201610093601 A CN201610093601 A CN 201610093601A CN 105733811 A CN105733811 A CN 105733811A
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- volatile oil
- graeci
- herba lysimachiae
- lysimachiae foenum
- aroma
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Classifications
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- A—HUMAN NECESSITIES
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- 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
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
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- A—HUMAN NECESSITIES
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- 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
- A24B15/307—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances of undetermined constitution characterised by their preparation using microorganisms or enzymes as catalysts
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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
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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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
Landscapes
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Abstract
一种葡萄糖苷酶促生香制备灵香草挥发油的方法，包括以下步骤：(1)将灵香草粗粉与水按质量比1:10～40混合，乙酸调pH至5～6，在45～55℃条件下平衡半小时，加入占灵香草粗粉质量比0.1～0.5％的β?葡萄糖苷酶混合均匀，并不停搅拌、45～55℃温育12～48小时；(2)水蒸气蒸馏5～10小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油。本发明经β?葡萄糖苷酶促生香，使灵香草的香味前体物经酶的作用产生降解、分解、转化生成丰富的、小分子的香气物质，而增加刺激感和杂气的物质含量减少甚至消失，将其在再造烟叶及低温卷烟中应用，可改善其未经酶促生香灵香草挥发油与烟气不协调、香气粗糙、刺激杂气大的缺陷。
Description
技术领域
本发明涉及烟用香料技术领域，具体是一种葡萄糖苷酶促生香制备灵香草挥发油的方法及其在再造烟叶和低温卷烟中的应用。
背景技术
再造烟叶，主要由烟末、碎片、烟梗或低次烟叶加入胶粘剂和其他添加剂等组成，存在杂气重、刺激性大和口感不适等吸味缺陷，影响了在卷烟产品中的使用效果和添加量。通常采用添加剂的办法来进行改善，目前应用较多的添加剂是烟草、天然植物类提取物或挥发油等，这些提取物一般通过水、醇提取、水蒸气蒸馏或分子蒸馏得到，添加后对卷烟质量的改善程度有限，仍有刺激性大、杂气多、香气不足等缺陷。
低温卷烟是一种运用碳质热源或电池电源等，在较低的温度(低于烟草点燃的温度700℃)下，加热挥发烟草香味物质并释放烟雾的低温卷烟，不含烟焦油，对人身体伤害较小，但也存在香气不足、口味效果不佳、抽吸感比不上传统卷烟产品的缺陷，影响了低温卷烟的品质，制约着低温卷烟的普及与流行。
灵香草报春花科珍珠菜属植物，拉丁学名Lysimachiafoenum-graecum Hance，全草含芳香油，可提炼香精、香脂香料；干品入箱中可防虫蛀衣物；又供药用，具散风寒、辟秽功效，治时邪感冒头痛、上气腰痛、胸闷腹胀、遗精、驱蛔虫等，是名贵的芳香植物。
本发明人在研究中发现：天然植物性香料中部分发香物质的发香基团往往容易与植物细胞中的其他成分如低分子的糖类等以化学键合的形式相结合，从而抑制了香味的散发并难以被提取在香料科学领域内将该类物质称为“香味前驱体”。这些物质本身并无香味且不挥发，但若选择合适的酶进行水解后，可释放出浓郁的具有天然特征香味的物质。
现有技术中，以灵香草为原料，采用葡萄糖苷酶促生香，制备灵香草挥发油，并在再造烟叶及低温卷烟中应用，改善烟气的香气质、口感，降低刺激减少杂气，尚未见报道。
发明内容
本发明针对现有技术的不足，提供一种酶促生香制备灵香草挥发油，经β-葡萄糖苷酶促生香，使灵香草的香味前体物经酶的作用产生降解、分解、转化生成丰富的、小分子的香气物质，而增加刺激感和杂气的物质含量减少甚至消失；以及该酶促生香灵香草挥发油在再造烟叶及低温卷烟中应用，改善其未经酶促生香灵香草挥发油与烟气不协调、香气粗糙、刺激杂气大的缺陷，而能与烟气协调，丰富香气、改善烟气的香气质、口感，降低刺激、减少杂气等。
本发明提供一种葡萄糖苷酶促生香制备灵香草挥发油的方法，包括以下步骤：
(1)将灵香草粗粉与水按质量比1:10～40混合，乙酸调pH至5～6，在45～55℃条件下平衡半小时，加入占灵香草粗粉质量比0.1～0.5％的β-葡萄糖苷酶混合均匀，并不停搅拌、45～55℃温育12～48小时；
(2)水蒸气蒸馏5～10小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油。
本发明提供一种上述方法制备的灵香草挥发油在再造烟叶中的应用，所述灵香草挥发油占烟丝的质量比为0.01～0.03％。
本发明提供一种上述方法制备的灵香草挥发油在低温卷烟中的应用，所述灵香草挥发油占电子烟烟液的质量比为0.01～0.03％；占碳加热卷烟雾化剂的质量比为1～5％，占碳加热卷烟烟丝的质量比为0.01～0.03％。
本发明对灵香草葡萄糖苷酶促生香挥发油与未经酶促生香的灵香草挥发油对照(以下简称对照)进行挥发性致香成分GC/MS进行对比。
(1)挥发油处理：将挥发油用二氯甲烷萃取、稀释100倍，取1～2mL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1)表明，①未经酶促生香处理的灵香草挥发油中共分离鉴定出42种挥发性香气成分，主要包括醇类、醛类、酮类、蒽、菲类、高级脂肪酸及高级脂肪酸酯类、烷烃和酚类；②经酶促生香的灵香草挥发油中共分离鉴定出64种挥发性香气成分；③经酶促生香的灵香草挥发油中新出现了40种香气成分，主要有右旋龙脑、十一烯醛、大马士酮、β-紫罗兰酮、肉豆蔻醛、(+)-白菖油萜、月桂酸、4-甲基二苯并呋喃、2-羟基-4,6-二甲氧基苯甲醛、十三酸、芴、9-芴醇、9-芴酮、呋喃、菲、金合欢基丙酮、亚油酸甲酯、亚麻酸甲酯等。其中，右旋龙脑又称冰片，有清香气和凉味，使喉部刺激感降低；十一烯醛，稀释后有强烈的玫瑰、柑橘型香气；大马士酮是萜烯类香气物质，有甜水果香气；β-紫罗兰酮香气较柔和而木香稍重，具有覆盆子的香味，被稀释以后有类似紫罗兰花和柏木香味；肉豆蔻醛具有脂肪香、蜡香、牛奶香、奶油香、鱼香、果香等；月桂酸是高级脂肪酸，存在于烤烟烟叶、烟气中，天然存在于月桂油中；酮类是烟气重要中性成分，金合欢基丙酮具有淡的青甜香气，增加青甜香和烤烟香；亚油酸甲酯、亚麻酸甲酯均为不饱和脂肪酸，是构成卷烟香味的重要物质，柔和烟气，减轻刺激；芳醛对卷烟加香有重要作用；④经酶促生香的灵香草挥发油中芳樟醇、α-萜品醇、茴香脑、棕榈酸等成分的含量有不同程度地提高。其中芳樟醇增加烟气的青香和木香；α-萜品醇具有优雅稳定持久的紫丁香香气，稀释后有桃似的甜味；茴香脑带有甜味,具茴香的特殊香气；棕榈酸能柔和卷烟烟气；⑤酶促生香后，灵香草挥发油中的一些成分消失或含量降低：十四烯醛、薄荷醇、十一醛、环庚烯、5-氨基-1-苯基吡唑、β-石竹烯、亚油酸、(+)-花侧柏烯、二苯并呋喃、十三醛、芴、氧化石竹烯、Z-3-十七烯、E-十四碳烯醇、5-亚硝基-5氢-二苯并[b，f]氮杂、邻苯二甲酸丁基烷基酯、十七酸、甲基菲、1,3,7,7-四甲基-2-氧杂环[4.4.0]-9-癸烯-8-酮、14-十五碳烯酸、正二十烷、2—氟苯甲酸辛-3-烯基-2-酯等，其中十七酸、十七烯、十一醛等成分可能带给卷烟烟气青草类杂气和刺激，在酶解后完全消失或含量显著下降，而有些如β-石竹烯(具有辛香、木香、柑橘香、樟脑香,温和的丁香香气)等物质相对百分含量减少，可能是经葡萄糖苷酶体系酶促生香，大分子物质断裂分解、降解，产生更多的小分子香气物质或者转化成别的挥发性香气成分甚至消失，可能有利于卷烟品质的提高。总之，从挥发、半挥发性成分的变化看，经酶促生香的灵香草挥发油在再造烟叶或低温卷烟中的加香效果可能比对照好。
表1葡萄糖苷酶促生香灵香草挥发油与其对照的挥发性成分GC/MS对比分析
表1中符号“－”表示未检出；内标为丙酸苯乙酯。
(4)在再造烟叶和低温卷烟中加香的感官评价分析
经过再造烟叶加香评吸试验(表2)表明，经酶促生香的灵香草挥发油在再造烟叶中的加香效果明显好于未酶促处理的灵香草挥发油(简称对照)，香气特征表现得更为突出，香气丰富、香气质提高，烟气更加柔和细腻，刺激性、杂气明显降低，适宜加香量为0.02％。
表2酶促生香灵香草挥发油及其对照样品在再造烟叶中的加香评吸结果
经过在电子烟烟液或碳加热雾化剂中加香，进行评吸试验(表3)表明，经酶促生香的灵香草挥发油在低温卷烟中的加香效果明显好于未酶促处理的灵香草挥发油(简称对照)，香气特征表现得更为突出，与烟香协调，香气质提高，烟气更加柔和细腻，刺激性、杂气降低，留香时间更长，适宜加香量为0.03％。
表3酶促生香灵香草挥发油及其对照样品在低温卷烟中的加香评吸结果
本发明的优点是：经葡萄糖苷酶对灵香草酶促生香提取挥发油，其挥发油的香气成分变化大，香气更丰富、香气质提高，带来刺激和杂气的挥发性物质消失或减少，大分子物质经酶促生香降解、分解、转化成小分子香气物质甚至消失；在再造烟叶和低温卷烟中应用，具有协调烟气、增加甜香、柔和舒适、降低刺激、减少杂气、改善吸味的优点，能与其它烟用香精香料混合调配使用，改善了未经酶解的灵香草挥发油在再造烟叶和低温卷烟中与烟气不协调、粗糙、刺激性大、杂气重的缺陷。该方法所用原料来源广泛，仪器简单，易于操作和实现产业化，成本低，绿色环保，旨在为酶促生香开发天然烟用香料的应用提供参考。
具体实施方式
下面列举一部分实施例对本发明的有关技术问题作进一步详细的描述，有必要在此指出以下具体实施例只是对本发明的进一步说明，不代表对本发明保护范围的限制。其他人根据本发明做出的一些非本质的修改和调整，仍属于本发明的保护范围。
实施例1
(1)将灵香草粗粉与水按质量比1:30混合，乙酸调pH至6，在50℃条件下平衡半小时，加入占灵香草粗粉质量比0.3％的β-葡萄糖苷酶混合均匀，并不停搅拌、50℃温育28小时；
(2)水蒸气蒸馏5小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油；
将上述灵香草酶促生香挥发油在再造烟叶中加香，占再造烟叶的质量比为0.01％。
感官评吸效果：与烟气协调性好，有清甜香，烟气柔和、刺激降低、杂气减少、余味干净，香气质提高。
实施例2
(1)将灵香草粗粉与水按质量比1:40混合，乙酸调pH至5.5，在45℃条件下平衡半小时，加入占灵香草粗粉质量比0.5％的β-葡萄糖苷酶混合均匀，并不停搅拌、45℃温育48小时；
(2)水蒸气蒸馏8小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油；
将上述灵香草酶促生香挥发油在电子烟烟液中加香，占电子烟烟液的质量比为0.01％。
感官评吸效果：与烟气协调性好，香气更丰富，香气质提高，烟气柔和细腻，刺激明显降低，杂气减少，余味干净。
实施例3
(1)将灵香草粗粉与水按质量比1:35混合，乙酸调pH至5，在55℃条件下平衡半小时，加入占灵香草粗粉质量比0.25％的β-葡萄糖苷酶混合均匀，并不停搅拌、55℃温育32小时；
(2)水蒸气蒸馏10小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油；
将上述灵香草酶促生香挥发油在碳加热卷烟雾化剂中加香，占雾化剂的质量比为5％，与碳加热卷烟烟丝的质量比为0.01％。
感官评吸效果：与烟气协调性好，带有甜香，烟气柔和、刺激降低、杂气减少、余味干净，香气质提高。
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 (3)
1.一种葡萄糖苷酶促生香制备灵香草挥发油的方法，其特征在于：包括以下步骤：
(1)将灵香草粗粉与水按质量比1:10～40混合，乙酸调pH至5～6，在45～55℃条件下平衡半小时，加入占灵香草粗粉质量比0.1～0.5％的β-葡萄糖苷酶混合均匀，并不停搅拌、45～55℃温育12～48小时；
(2)水蒸气蒸馏5～10小时提取挥发油，所得黄绿色油状物为酶促生香灵香草挥发油。
2.一种如权利要求1所述的方法制备的灵香草挥发油在再造烟叶中的应用，所述灵香草挥发油占烟丝的质量比为0.01～0.03％。
3.一种如权利要求1所述的方法制备的灵香草挥发油在低温卷烟中的应用，所述灵香草挥发油占电子烟烟液的质量比为0.01～0.03％；占碳加热卷烟雾化剂的质量比为1～5％，占碳加热卷烟烟丝的质量比为0.01～0.03％。
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| CN102150948A (zh) * | 2011-05-19 | 2011-08-17 | 湖北中烟工业有限责任公司 | 一种烟用茉莉花提取物的制备方法 |
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| CN101457178A (zh) * | 2008-12-10 | 2009-06-17 | 广西中烟工业有限责任公司 | 一种从灵香草中提取水溶性挥发油的方法 |
| CN102150948A (zh) * | 2011-05-19 | 2011-08-17 | 湖北中烟工业有限责任公司 | 一种烟用茉莉花提取物的制备方法 |
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| CN108315352A (zh) * | 2018-01-31 | 2018-07-24 | 湖北中烟工业有限责任公司 | 一种酶促生香制备薰衣草油的方法及其应用 |
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