粉状烟草提取物的制备及在胶基型嚼烟中的应用
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摘要
为制备在胶基型嚼烟中具有广泛适用性的粉状烟草提取物,优化了喷雾干燥法的工艺参数,采用顶空-固相微萃取-气相色谱/质谱法(HS-SPME-GC/MS)检测津巴布韦烟草提取物中挥发性致香成分,并结合主成分分析法(PCA)建立了不同批次粉状烟草提取物的均质化评价方法。结果表明:(1)确定的制备工艺参数为进料流量500 mL/h,进风温度200℃,在此条件下粉状烟草提取物的得率为44.55%(含水率6.02%)。(2)使用Blue fiber萃取头在80℃下萃取30 min后,可从粉末中检测出36种挥发性致香成分,其中烟碱含量(质量分数)最高,为52.14%,茄酮、西柏三烯二醇和巨豆三烯酮的含量分别为14.22%、3.91%和3.89%。(3)在3%用量下,制备的粉状烟草提取物能够显著提升胶基型嚼烟的烟草本香,且劲头适中。该方法适用于粉状烟草提取物的质量稳定性评价。
In order to obtain a powdered tobacco extract with broad applicability in gum-based chewing tobacco,the parameters of spray-drying process were optimized. The volatile aroma components in the extract of a Zimbabwe tobacco were analysed by headspace-solid phase microextraction-gas chromatography/mass spectrometry(HS-SPME-GC/MS) combined with principal component analysis(PCA). A method for homogenization evaluation of different batches of dry tobacco extract powder was also established. The results showed that: 1) The optimal preparation parameters were feeding flow 500 mL/h and inlet air temperature200 ℃, the yield of dry powder from the tobacco extract(with a moisture content of 6.02%)reached 44.55%under the condition. 2) After extracting for 30 min at 80 ℃ with a Blue fiber extraction head, 36 volatile components were detected in the dry powder. Among them, the nicotine content(mass fraction)was the highest(52.14%), and the contents of solanone, cymbriatrienediol and megastigmatrienone were 14.22%, 3.91% and3.89%, respectively. 3) At an addition level of 3%, the dry powder prepared from the tobacco extract significantly improved tobacco-like aroma of a gum-based chewing tobacco with a moderate strength. This method is suitable for evaluating the quality consistency of powdered tobacco extract.
In order to obtain a powdered tobacco extract with broad applicability in gum-based chewing tobacco,the parameters of spray-drying process were optimized. The volatile aroma components in the extract of a Zimbabwe tobacco were analysed by headspace-solid phase microextraction-gas chromatography/mass spectrometry(HS-SPME-GC/MS) combined with principal component analysis(PCA). A method for homogenization evaluation of different batches of dry tobacco extract powder was also established. The results showed that: 1) The optimal preparation parameters were feeding flow 500 mL/h and inlet air temperature200 ℃, the yield of dry powder from the tobacco extract(with a moisture content of 6.02%)reached 44.55%under the condition. 2) After extracting for 30 min at 80 ℃ with a Blue fiber extraction head, 36 volatile components were detected in the dry powder. Among them, the nicotine content(mass fraction)was the highest(52.14%), and the contents of solanone, cymbriatrienediol and megastigmatrienone were 14.22%, 3.91% and3.89%, respectively. 3) At an addition level of 3%, the dry powder prepared from the tobacco extract significantly improved tobacco-like aroma of a gum-based chewing tobacco with a moderate strength. This method is suitable for evaluating the quality consistency of powdered tobacco extract.
引文
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[20]Q/YNZY.J05.003-2017粒状胶基型嚼烟生产工艺[S].Q/YNZY.J05.003-2017 Production process of granular gum-based chewing tobacco[S].
[21]Q/YNZY.J07.002-2014无烟气烟草制品胶基型嚼烟感官评价方法[S].Q/YNZY.J07.002-2014 Smokeless tobacco productsGum-based chewing tobacco-Sensory evaluation methods[S].
[22]刘春泉,宋江峰,章英,等.甘薯叶提取物喷雾干燥工艺研究[J].食品科学,2011,32(6):45-48.LIU Chunquan,SONG Jiangfeng,ZHANG Ying,et al.Spray drying of sweet potato leaf extract[J].Food Science,2011,32(6):45-48.
[23]Orunaconcha M J,Duckham S C,Ames J M.Comparison of volatile compounds isolated from the skin and flesh of four potato cultivars after baking[J].Journal of Agricultural and Food Chemistry,2001,49(5):2414-2421.
[24]戴魁,李诗平,王文斌,等.模拟红薯烘烤制备焦甜香香料及其卷烟应用[J].烟草科技,2015,48(9):27-32,44.DAI Kui,LI Shiping,WANG Wenbin,et al.Preparation of flavor with burnt-sweetness scent by simulating sweet potato roasting and its application to cigarette[J].Tobacco Science&Technology,2015,48(9):27-32,44.
[25]杨鹏元,洪广峰,马宇平,等.焦麦芽烤甜香关键成分的确定及制备工艺优化[J].中国烟草科学,2016,37(5):68-74.YANG Pengyuan,HONG Guangfeng,MA Yuping,et al.Determination of key components of the roasted sweet aroma in burnt malt extracts and optimization of its preparation process[J].Chinese Tobacco Science,2016,37(5):68-74.
[26]黄龙,朱巍,程志昆,等.红枣提取物的Maillard反应制备烟用香料的研究[J].湖北农业科学,2011,50(8):1673-1676.HUANG Long,ZHU Wei,CHENG Zhikun,et al.Research on Maillard reaction product of Ziziphus jujuba extract and its application in tobacco[J].Hubei Agricultural Sciences,2011,50(8):1673-1676.
[27]刘芳,杨柳,倪朝敏,等.超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚[J].烟草科技,2007(10):31-35.LIU Fang,YANG Liu,NI Chaomin,et al.Determination of phenol,cresols,and dihydroxybenzenes in mainstream cigarette smoke with ultrasonic extraction and fast HPLC[J].Tobacco Science&Technology,2007(10):31-35.
[28]谢复炜,赵明月,王昇,等.卷烟主流、侧流烟气中酚类化合物的高效液相色谱测定[J].烟草科技,2004(5):6-10.XIE Fuwei,ZHAO Mingyue,WANG Sheng,et al.High performance liquid chromatographic determination of major phenolic compounds in mainstream and sidestream cigarette smoke[J].Tobacco Science&Technology,2004(5):6-10.
[29]黄朝章.超高效液相色谱快速测定卷烟主流烟气中7种挥发酚[J].烟草科技,2011(8):44-47.HUANG Chaozhang.Fast analysis of 7 volatile phenols in mainstream cigarette smoke with ultra performance liquid chromatography[J].Tobacco Science&Technology,2011(8):44-47.
[30]杨金初,郝辉,马宇平,等.甘薯浸膏的开发及其香气成分分析[J].中国烟草学报,2016,22(5):10-18.YANG Jinchu,HAO Hui,MA Yuping,et al.Development of sweet potato extract and its flavor components analysis[J].Acta Tabacaria Sinica,2016,22(5):10-18.
[2]Azarmi S,Roa W,L?benberg R.Current perspectives in dissolution testing of conventional and novel dosage forms[J].International Journal of Pharmaceutics,2007,328(1):12-21.
[3]刘亚丽,孙世豪,郑新章,等.基于专利数据分析的无烟气烟草制品研发趋势研究[J].中国烟草学报,2010,16(5):35-38.LIU Yali,SUN Shihao,ZHENG Xinzhang,et al.An overview of research and development in smokeless tobacco products based on patent data analysis[J].Acta Tabacaria Sinica,2010,16(5):35-38.
[4]Hatsukami D K,Ebbert J O,Feuer R M,et al.Changing smokeless tobacco products:new tobaccodelivery systems[J].American Journal of Preventive Medicine,2007,33(6):S368-S378.
[5]Centers for Disease Control and Prevention.Determination of nicotine,p H,and moisture content of six US commercial moist snuff products-Florida,January-February 1999[J].JAMA,1999,281(24):2279-2280.
[6]US Food and Drug Administration.Nicotine in cigarettes and smokeless tobacco is a drug and these products are nicotine delivery devices under the Federal Food,Drug,and Cosmetic Act:jurisdictional determination[J].Federal Register,1996,61:44619-45381.
[7]韩敬美,汤建国,袁大林,等.HS/GC-MS法分析胶基型嚼烟中的挥发性香味物质[J].分析测试学报,2016,35(8):1005-1009.HAN Jingmei,TANG Jianguo,YUAN Dalin,et al.Analysis of volatile flavor components in tobacco chewing gum by headspace/GC-MS[J].Journal of Instrumental Analysis,2016,35(8):1005-1009.
[8]Djordjevic M V,Hoffmann D,Glynn T,et al.UScommercial brands of moist snuff,1994.I.Assessment of nicotine,moisture,and pH[J].Tobacco Control,1995,4(1):62-66.
[9]Nasr M M,Reepmeyer J C,Tang Y.In vitro study of nicotine release from smokeless tobacco[J].Journal of AOAC International,1998,81(3):540-543.
[10]张文娟,何保江,屈展,等.胶基型无烟气烟草制品中烟碱的释放行为研究[J].烟草科技,2013(6):31-36.ZHANG Wenjuan,HE Baojiang,QU Zhan,et al.Evaluation of release behavior of nicotine from gum-based tobacco products[J].Tobacco Science&Technology,2013(6):31-36.
[11]张杰,李鹏,宗永立,等.国外口含型无烟气烟草制品总烟碱、游离烟碱和烟草特有亚硝胺含量分析[J].烟草科技,2011(10):44-48.ZHANG Jie,LI Peng,ZONG Yongli,et al.Analysis of total nicotine,free nicotine and tobacco-specific N-nitrosamines in foreign oral smokeless tobacco products[J].Tobacco Science&Technology,2011(10):44-48.
[12]Toelstede S,Dunkel A,Hofmann T.A series of kokumi peptides impart the long-lasting mouthfulness of matured Gouda cheese[J].Journal of Agricultural and Food Chemistry,2009,57(4):1440-1448.
[13]张明福,张建平.烟草二氧化碳超临界萃取物的初步研究[J].烟草科技,2001(8):24-27.ZHANG Mingfu,ZHANG Jianping.Preliminary study on carbon dioxide supercritical fluid extraction of tobacco[J].Tobacco Science&Technology,2001(8):24-27.
[14]常乃杰,张云贵,刘青丽,等.应用SPSS软件研究典型中间香型烤烟常规化学成分与烟气成分的关系[J].烟草科技,2017,50(4):31-36.CHANG Naijie,ZHANG Yungui,LIU Qingli,et al.Relationships between routine leaf chemical components in typical medium flavor flue-cured tobacco and mainstream cigarette smoke components by SPSS[J].Tobacco Science&Technology,2017,50(4):31-36.
[15]李超,刘秀明,秦云华,等.基于挥发性特征组分的卷烟烟丝质量趋势分析[J].烟草科技,2017,50(11):39-47.LI Chao,LIU Xiuming,QIN Yunhua,et al.Quality trend analysis on cigarette cut filler based on characteristic volatile components in cut filler[J].Tobacco Science&Technology,2017,50(11):39-47.
[16]刘熠宇,包秀萍,王松峰,等.一种烟草精油的制备方法:CN102499465A[P].2012-06-20.LIU Yiyu,BAO Xiuping,WANG Songfeng,et al.Preparation method of tobacco essence:CN102499465A[P].2012-06-20.
[17]蒋美红,刘煜宇,念小魁,等.土耳其香料烟中关键组分的制备及分析[J].精细化工,2010,27(3):248-253.JIANG Meihong,LIU Yuyu,NIAN Xiaokui,et al.Preparation and analysis of key components of Turkish tobacco[J].Fine Chemicals,2010,27(3):248-253.
[18]杨乾栩,冯斌,吴长伟,等.基于大孔树脂静态吸附的烟草增香组分制备及应用[J].烟草科技,2014(10):39-44.YANG Qianxu,FENG Bin,WU Changwei,et al.Preparation and application of tobacco flavor-enhancing fraction based on static adsorption of macroporous resins[J].Tobacco Science&Technology,2014(10):39-44.
[19]胡建军,周冀衡,李文伟,等.烤烟香味成分与其感官质量的典型相关分析[J].烟草科技,2007(3):9-15,22.HU Jianjun,ZHOU Jiheng,LI Wenwei,et al.Canonical correlation between flavor components and smoking quality of flue-cured tobacco[J].Tobacco Science&Technology,2007(3):9-15,22.
[20]Q/YNZY.J05.003-2017粒状胶基型嚼烟生产工艺[S].Q/YNZY.J05.003-2017 Production process of granular gum-based chewing tobacco[S].
[21]Q/YNZY.J07.002-2014无烟气烟草制品胶基型嚼烟感官评价方法[S].Q/YNZY.J07.002-2014 Smokeless tobacco productsGum-based chewing tobacco-Sensory evaluation methods[S].
[22]刘春泉,宋江峰,章英,等.甘薯叶提取物喷雾干燥工艺研究[J].食品科学,2011,32(6):45-48.LIU Chunquan,SONG Jiangfeng,ZHANG Ying,et al.Spray drying of sweet potato leaf extract[J].Food Science,2011,32(6):45-48.
[23]Orunaconcha M J,Duckham S C,Ames J M.Comparison of volatile compounds isolated from the skin and flesh of four potato cultivars after baking[J].Journal of Agricultural and Food Chemistry,2001,49(5):2414-2421.
[24]戴魁,李诗平,王文斌,等.模拟红薯烘烤制备焦甜香香料及其卷烟应用[J].烟草科技,2015,48(9):27-32,44.DAI Kui,LI Shiping,WANG Wenbin,et al.Preparation of flavor with burnt-sweetness scent by simulating sweet potato roasting and its application to cigarette[J].Tobacco Science&Technology,2015,48(9):27-32,44.
[25]杨鹏元,洪广峰,马宇平,等.焦麦芽烤甜香关键成分的确定及制备工艺优化[J].中国烟草科学,2016,37(5):68-74.YANG Pengyuan,HONG Guangfeng,MA Yuping,et al.Determination of key components of the roasted sweet aroma in burnt malt extracts and optimization of its preparation process[J].Chinese Tobacco Science,2016,37(5):68-74.
[26]黄龙,朱巍,程志昆,等.红枣提取物的Maillard反应制备烟用香料的研究[J].湖北农业科学,2011,50(8):1673-1676.HUANG Long,ZHU Wei,CHENG Zhikun,et al.Research on Maillard reaction product of Ziziphus jujuba extract and its application in tobacco[J].Hubei Agricultural Sciences,2011,50(8):1673-1676.
[27]刘芳,杨柳,倪朝敏,等.超声萃取-快速HPLC法测定卷烟主流烟气中的苯酚、甲酚和苯二酚[J].烟草科技,2007(10):31-35.LIU Fang,YANG Liu,NI Chaomin,et al.Determination of phenol,cresols,and dihydroxybenzenes in mainstream cigarette smoke with ultrasonic extraction and fast HPLC[J].Tobacco Science&Technology,2007(10):31-35.
[28]谢复炜,赵明月,王昇,等.卷烟主流、侧流烟气中酚类化合物的高效液相色谱测定[J].烟草科技,2004(5):6-10.XIE Fuwei,ZHAO Mingyue,WANG Sheng,et al.High performance liquid chromatographic determination of major phenolic compounds in mainstream and sidestream cigarette smoke[J].Tobacco Science&Technology,2004(5):6-10.
[29]黄朝章.超高效液相色谱快速测定卷烟主流烟气中7种挥发酚[J].烟草科技,2011(8):44-47.HUANG Chaozhang.Fast analysis of 7 volatile phenols in mainstream cigarette smoke with ultra performance liquid chromatography[J].Tobacco Science&Technology,2011(8):44-47.
[30]杨金初,郝辉,马宇平,等.甘薯浸膏的开发及其香气成分分析[J].中国烟草学报,2016,22(5):10-18.YANG Jinchu,HAO Hui,MA Yuping,et al.Development of sweet potato extract and its flavor components analysis[J].Acta Tabacaria Sinica,2016,22(5):10-18.