CN106978258A - 酶促增香提高香气品质的杭白菊挥发油的制备方法及应用 - Google Patents
酶促增香提高香气品质的杭白菊挥发油的制备方法及应用 Download PDFInfo
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- CN106978258A CN106978258A CN201710371606.XA CN201710371606A CN106978258A CN 106978258 A CN106978258 A CN 106978258A CN 201710371606 A CN201710371606 A CN 201710371606A CN 106978258 A CN106978258 A CN 106978258A
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- flos chrysanthemi
- china
- chrysanthemi alba
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- 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
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Abstract
本发明提供一种酶促增香提高香气品质的杭白菊挥发油的制备方法，具体来说是采用复合酶(β‑葡萄糖苷酶、风味蛋白酶)发酵预处理杭白菊花，分解、降解、转化杭白菊花细胞壁大分子物质，在水溶液中释放更多致香物质，水蒸气蒸馏提取杭白菊挥发油，经复合酶促增香提高杭白菊挥发油香气品质，丰富香气，具有菊花、玫瑰花复合香气，喉部有甜感和微清凉感；在卷烟中加香应用，改善烟气的香气质、口感，降低刺激，柔和烟气，丰富烟香。
Description
技术领域
本发明涉及烟用添加剂技术领域，具体是一种酶促增香提高香气品质的杭白菊挥发油的制备方法及其应用。
背景技术
烟用香料是伴随卷烟工业发展而出现的产物，是高、精、新技术的结晶。提高卷烟安全性，降低烟气焦油量和烟气中其它有害成分是中式卷烟研究的一个重要方向。然而，烟草中的许多香味物质却存在于焦油之中，伴随着焦油量的降低，烟味变淡，香气减弱，卷烟产品失去原有的风格，难以被消费者所接受。因此，在降低卷烟焦油的同时，增进和提高烟气浓度和香味、稳定卷烟质量，满足个性化需要，提高安全性等诸多方面，加香加料都具重要作用。随着中式卷烟降焦减害工作的深入，烟草加香加料愈加显示出其重要性。
杭白菊(HangZhou White Chrysanthemum)，又名杭菊、甘菊、茶菊，产自浙北杭嘉湖平原以桐乡市为主，按照传统工艺技术在当地加工而成。杭白菊既可作饮料，又是重要的中药材，是“浙八味”之一，素有“西湖龙井，杭白贡菊”之美誉；其成品外观花瓣玉白、花蕊深黄，花型较大，花瓣厚实，花朵大小均匀，用开水冲泡后卤汁澄清，呈浅黄色，气清香、味甘微苦。杭白菊具有疏风散热、解毒清肿、利咽明目、降低血压的作用；研究表明，杭白菊提取物可以增强毛细血管抵抗力，降低血液中脂肪和胆固醇含量，具有改善心肌营养、抗炎的作用；具有清除活性氧自由基，对抑制肿瘤、延缓衰老及增强人体免疫力有一定功效。
β-葡萄糖苷酶，又称β-D-葡萄糖苷葡萄糖水解酶，它能够水解结合于末端非还原性的β-D-葡萄糖苷键，同时释放出β-D-葡萄糖和相应的配基。β-葡萄糖苷酶能将果、蔬、茶中的风味前体物质水解为具有浓郁天然风味的香气物质，还能协助纤维素酶降解纤维素。
风味蛋白酶(Flavourzyme)是利用米曲霉发酵提取而得，筛选复配而成的复合酶。包含了内切蛋白酶与外切肽酶两种活性,可以用来去除低水解度产物的苦肽链，将其彻底降解为氨基酸，也可以用于彻底水解蛋白质，增进和改善水解液的风味。
现有技术中，以β-葡萄糖苷酶和风味蛋白酶复合发酵预处理杭白菊花，分解、降解、转化杭白菊花细胞壁大分子物质，提高杭白菊挥发油香气品质，并在卷烟中加香应用，改善烟气的香气质、口感，尚未见报道。
发明内容
本发明针对现有技术的不足，提供一种酶促增香提高香气品质的杭白菊挥发油的制备方法，具体来说是采用复合酶(β-葡萄糖苷酶、风味蛋白酶)发酵预处理杭白菊花，分解、降解、转化杭白菊花细胞壁大分子物质，在水溶液中释放更多致香物质，水蒸气蒸馏提取杭白菊挥发油，经复合酶促增香提高杭白菊挥发油香气品质，丰富香气，具有菊花、玫瑰花复合香气，喉部有甜感和微清凉感；在卷烟中加香应用，改善烟气的香气质、口感，降低刺激，柔和烟气，丰富烟香。
本发明提供一种酶促增香提高香气品质的杭白菊挥发油的制备方法，包括以下步骤：
(1)将杭白菊花与水按质量比1:25～50混合，调pH至4～6，加入混合物总质量3～6％的乙醇，在35～50℃条件下平衡10～30min，加入占杭白菊花质量比0.1～0.3％的复合酶，混合均匀并不停搅拌、35～50℃温育12～48小时，所述复合酶由β-葡萄糖苷酶和风味蛋白酶按照质量比0.5～2:1组成；
(2)水蒸气蒸馏5～10小时提取挥发油，所得黄色油状物为酶促增香提高香气品质的杭白菊挥发油。
进一步的，所述的β-葡萄糖苷酶为食品级，酶活为100～10000u/g。
进一步的，所述的风味蛋白酶为食品级，酶活为1万～5万u/g。
进一步的，所述的乙醇为食品级，质量浓度为95％。
本发明提供一种上述方法制备的杭白菊挥发油。
本发明提供一种上述方法制备的杭白菊挥发油在卷烟中的应用，将所述杭白菊挥发油按质量比百万分之0.1～0.3添加到烟丝中。
本发明的优点：采用复合酶(β-葡萄糖苷酶、风味蛋白酶)发酵预处理杭白菊花，其中β-葡萄糖苷酶水解结合于末端非还原性的β-D-葡萄糖苷键，同时释放出β-D-葡萄糖和相应的配基，将风味前体物质水解为香气物质，而包含内切蛋白酶和外切肽酶两种活性的风味蛋白酶，可以更彻底地水解蛋白质，破解细胞壁物质，利于致香成分的释放；而混合物3～6％含量的乙醇，是为了一定程度地提高β-葡萄糖苷酶的活性；在一定的温度、时间、复合酶的作用下，杭白菊花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，获取的杭白菊花挥发油，除了有菊花的特征香气成分，香气种类更丰富，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；在卷烟中加香，与烟气协调，具有丰富的菊花、玫瑰花香、甜和凉感，克服了增大刺激、有杂气的缺陷。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
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
一种酶促增香提高香气品质的杭白菊挥发油的制备方法，包括以下步骤：
(1)将杭白菊花与水按质量比1:25混合，调pH至4，加入混合物总质量3％的食品级95％乙醇，在35℃条件下平衡10min，加入占杭白菊花质量比0.1％的复合酶(，混合均匀并不停搅拌、35℃温育12小时，所述复合酶由β-葡萄糖苷酶和风味蛋白酶按照质量比为1:1组成；
(2)水蒸气蒸馏5小时提取挥发油，所得黄色油状物为酶促增香提高香气品质的杭白菊挥发油。
所述的β-葡萄糖苷酶为食品级，酶活为10000u/g。
所述的风味蛋白酶为食品级，酶活为3万u/g。
所述的乙醇为食品级，质量浓度为95％。
将上述杭白菊酶促生香挥发油在卷烟中加香，占烟丝质量比为百万分之0.1％。
感官评吸效果：与烟气协调性较好，有菊花特征香气，有清甜香，香气丰富，除了菊花特征香气，还具有玫瑰花香、甜感，并有喉部清凉感，烟气柔和，余味干净，香气质提高。
实施例2
一种酶促增香提高香气品质的杭白菊挥发油的制备方法，包括以下步骤：
(1)将杭白菊粗粉与水按质量比1:35混合，调pH至5.2，加入混合物总质量4.5％的食品级95％乙醇，在40℃条件下平衡20min，加入占杭白菊粗粉质量比0.3％的复合酶混合均匀，并不停搅拌、40℃温育18小时，所述复合酶由β-葡萄糖苷酶和风味蛋白酶按照质量比为0.5：1组成；
(2)水蒸气蒸馏6小时提取挥发油，所得黄色油状物为酶促生香杭白菊挥发油；
所述的β-葡萄糖苷酶为食品级，酶活为5000u/g。
所述的风味蛋白酶为食品级，酶活为2万u/g。
将上述杭白菊酶促生香挥发油在卷烟中加香，占烟丝质量比为百万分之0.2％。感官评吸效果：与烟气协调性好，香气丰富，具有丰富的菊花香气和玫瑰香，还有甜感和微清凉感，香气质提高，喉部舒适，烟气柔和细腻，刺激降低，余味干净。
实施例3
一种酶促增香提高香气品质的杭白菊挥发油的制备方法，包括以下步骤：
(1)将杭白菊粗粉与水按质量比1:45混合，调pH至6，加入混合物总质量6％的食品级95％乙醇，在48℃条件下平衡30min，加入占杭白菊粗粉质量比0.3％的复合酶(β-葡萄糖苷酶、风味蛋白酶)混合均匀，并不停搅拌、48℃温育32小时，所述复合酶由β-葡萄糖苷酶和风味蛋白酶按照质量比为1：0.5组成；
(2)水蒸气蒸馏12小时提取挥发油，所得黄色油状物为酶促生香杭白菊挥发油；
所述的β-葡萄糖苷酶为食品级，酶活为1000u/g。
所述的风味蛋白酶为食品级，酶活为1万u/g。
将上述杭白菊挥发油在卷烟中加香，占烟丝质量比为百万分之0.3％。
感官评吸效果：与烟气协调性好，具有菊花、玫瑰花香和甜、凉感，烟气柔和舒适、刺激降低、杂气减少、余味干净，香气质提高。
试验例1
本发明对酶促增香的杭白菊挥发油与其对照(未经酶预处理的杭白菊花水蒸气蒸馏提取的挥发油)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50:1；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未经酶发酵处理的杭白菊挥发油中共分离鉴定出106种挥发性香气成分，主要包括烯类、萜烯类、环烃族化合物、萜类醇类、酮类、醛类、烷烃类、萜烯类、，还有呋喃、吡嗪、噻吩等杂环类化合物，占78.23％，其中相对百分含量较高的几种物质分别为；1,2,4-三乙苯(13.89％)、α-姜黄烯(8.94％)、β-倍半水芹烯(6.04％)、(+)-δ-杜松烯(4.05％)、(-)-氧化石竹烯(3.14％)、.α.-杜松醇(2.70％)、1,2,3,4,4a,7-六氢-1,6-二甲基-4-(甲基乙基)-萘(2.12％)、姜烯(1.95％)、β-石竹烯(1.91％)等9种，共达44.74％；②经复合酶促生香的杭白菊挥发油中共分离鉴定出166种挥发性香气成分，相对百分含量占92.19％，其中α-姜黄烯(7.29％)、1,2,4-三乙苯(6.23％)、β-倍半水芹烯(5.16％)、(+)-δ-杜松烯(3.88％)、(S)-顺式-马鞭草烯醇(3.11％)、(-)-氧化石竹烯(2.69％)、γ-桉叶油(2.51％)、二-epi-.α.柏木烯(2.43％)、5-乙基环戊-1-烯吡咯甲醛(2.00％)、(E)-2,3-环氧皆烷(1.85％)、姜烯(1.78％)等11种香气物质相对百分含量较高，共达38.93％；
②经复合酶促发酵生香后，杭白菊挥发油中的香气成分更丰富，出现了新的香气成分101种，主要有苯甲醛、甲基庚烯酮、苯乙醛、苯乙醇、β-异佛尔酮、(+)-薄荷醇(0.71％)、香叶醇、橙花醇、水芹醛、(-)-乙酸桃金娘烯酯、(-)-α-古芸烯、(-)-罗汉柏烯、(+)-δ-杜松萜烯、(-)-α-柏木烯(0.34％)、(S)-顺式-马鞭草烯醇(3.11％)、β-桉叶醇(1.11％)、二-epi-.α.柏木烯(2.43％)、.tau.-杜松醇(1.17％)、香树烯(0.46％)、Z-.α.-trans-香柠檬醇(1.40％)、金合欢醇异构体(1.18％)、2-己基吡啶(1.34％)(+)-雪松醇(0.38％)、长马鞭草烯酮(0.52％)及其他呋喃、咪唑等。(S)-顺式-马鞭草烯醇具有马鞭草样香气，二-epi-.α.柏木烯有木香香气，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，4-伞花烃具特殊的香气，β-异佛尔酮有薄荷香味，苯乙醛具有类似风信子的香气，稀释后具行水果的甜香气，苯乙醇具有柔和、愉快而持久的玫瑰香气，(+/-)-薄荷醇具有薄荷香气并有清凉的作用，乙酸龙脑酯有清凉的松木香气，并有樟脑似的气息，橙花醇具有新鲜的、甜香的玫瑰似的香气，香叶醇具有温和、甜的玫瑰花气息，味有苦感，水芹醛有果子香味，(-)-罗汉柏烯具柏木特征香气，(+)-δ-杜松萜烯为萜烯类物质，(+)-雪松醇是一种倍半萜醇，具有愉快而持久的柏木香气，长马鞭草烯酮具有类似樟脑、薄荷脑、芹菜香气，金合欢醇异构体具有特有的青香韵的铃兰花香气,并有青香和木香香韵，亚油酸甲酯为不饱和脂肪酸，是构成卷烟香味的重要物质，柔和烟气，减轻刺激，微量亚油酸(0.01％)为醇和烟气成分；
③经复合酶促生香的杭白菊挥发油中，23种挥发性成分的相对百分含量提高，如(+,-)-1,3,3,-三甲基环己烯-4-吡咯甲醛、(-)-反式一松香芹醇、马鞭烯醇、1,3-环庚二烯、(1R,5R)-rel-香芹醇、(E)-2,3-环氧皆烷、(-)-α-荜澄茄油烯、γ-桉叶油、8,9-脱氢-环异长叶烯、cis-Z-.α.-红没药烯环氧化物、3’-甲基-2-苄叉-苯并二氢呋喃-3-酮、可巴烯等，其中马鞭烯醇具有马鞭草样香气，8、9-脱氢-环异长叶烯为单萜含氧化合物，具有类玫瑰花香气，cis-Z-.α.-红没药烯环氧化物具有温暖的木香、柑橘香、花香、果香、青香，和甜润的香脂香气，(-)-α-荜澄茄油烯有轻淡的樟木香气等；
④复合酶促生香后，杭白菊挥发油中的一些成分消失或含量降低：1,6-二甲基庚-1,3,5-三烯、异佛尔酮、L(-)-樟脑、1,4-二乙基-1,4-二甲基-2，5-环己二烯、薄荷脑、(-)-4-萜品醇、β-甲基苯丙醛、1,1,6-三甲基四啉、左旋乙酸冰片酯、6,7-二甲基-1,2,3,5,8,8a-六氢萘、1,2,3,4-四甲基苯、长叶烯-(V4)、丁香酚、正癸酸、1-乙基-3-甲基金刚烷、1，2,3,4-四氢-1,5,7-三甲基萘、4-乙基邻二甲苯、2-异丙烯基-2-长松针烯、2，6-二甲基-6-(4-甲基-3-戊烯基)双环[3.1.1]庚-2-烯、(+)-δ-杜松烯、(1.α.,3.α.,5.α.)-1,5-二乙烯-3-甲基-2-亚甲基环己烷、(R*,R*)-4-甲基-.α.-(1-甲基-2-丙烯基)-苯甲醇、邻甲苯酸十三烷酯、10,10-二甲基-2,6-二甲烯双环[7.2.0]十一-5.β.-醇等，其中1,2,4-三乙苯的相对百分含量，从13.89％降至6.23％，共12种含量降低，35种消失，这些杂环烯烃、杂环化合物、醇、酯等，可能是在β-葡萄糖苷酶的作用下，有些成分发生了结构变化形成了同分异构体，有些发生了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香味前体物质，有些彻底降解而消失，使刺激性成分减少，可能有利于卷烟品质的提高。
总的来看，所有这些香气成分赋予酶促生香的杭白菊挥发油，除了有菊花的特征香气成分，香气种类更丰富，具有了玫瑰花香、果甜香、微凉感等复合天然气息，香气质提高；在卷烟中加香，与烟气协调，具有丰富的菊花、玫瑰花香、甜和凉感，刺激性降低，余味干净。
表1β-葡萄糖苷酶发酵提取杭白菊挥发油与其对照的挥发性成分GC/MS对比
表1中符号“/”表示未检出；丙酸苯乙酯为内标。
试验例2在卷烟中加香的感官评价分析
将实施例1-3酶促生香提高香气品质的杭白菊挥发油按烟丝质量比的百万分之0.1分别添加到某中档卷烟品牌配方烟丝中，烟丝装入密封袋，放置在烘箱中80℃恒温30min，至含水量合适，卷制成烟支，放入恒温恒湿箱内(22℃+1、相对湿度为60％+2％)平衡48h，请专家评吸小组评吸。
经过经评吸小组反复评吸，卷烟评吸试验(表2)表明，经酶促生香的杭白菊挥发油在烟丝中的加香效果明显好于未酶促处理的杭白菊挥发油(简称对照)，香气特征表现得更为丰富，具有菊花特征香气的同时，还带有玫瑰花香和甜感、喉部微清凉感，烟气柔和，刺激性、杂气明显降低，香气品质提高。
表2酶促增香提高香气品质的杭白菊挥发油及其对照的感官评吸结果
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 (6)
1.一种酶促增香提高香气品质的杭白菊挥发油的制备方法，其特征在于包括以下步骤：
(1)将杭白菊花与水按质量比1:25～50混合，调pH至4～6，加入混合物总质量3～6％的乙醇，在35～50℃条件下平衡10～30min，加入占杭白菊花质量比0.1～0.3％的复合酶，混合均匀并不停搅拌、35～50℃温育12～48小时，所述复合酶由β-葡萄糖苷酶和风味蛋白酶按照质量比0.5～2:1组成；
(2)水蒸气蒸馏5～10小时提取挥发油，所得黄色油状物为酶促增香提高香气品质的杭白菊挥发油。
2.如权利要求1所述的酶促增香提高香气品质的杭白菊挥发油的制备方法，其特征在于：所述的β-葡萄糖苷酶为食品级，酶活为100～10000u/g。
3.如权利要求1所述的酶促增香提高香气品质的杭白菊挥发油的制备方法，其特征在于：所述的风味蛋白酶为食品级，酶活为1万～5万u/g。
4.如权利要求1所述的酶促增香提高香气品质的杭白菊挥发油的制备方法，其特征在于：所述的乙醇为食品级，质量浓度为95％。
5.一种如权利要求1-4中任一项所述方法制备的杭白菊挥发油。
6.一种如权利要求1-4中任一项所述方法制备的杭白菊挥发油在卷烟中的应用，将所述杭白菊挥发油按质量比百万分之0.1～0.3添加到烟丝中。
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Application publication date: 20170725 |