广佛手精油微胶囊制备工艺优化及其品质分析
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摘要
以广佛手精油为原料,对其微胶囊的制备工艺包括壁材组合、乳化工艺(乳化剂组成及用量、芯壁比)及喷雾干燥条件(进风温度、雾化器频率、进料流量)进行了优化研究,确定最优的微胶囊化工艺参数,进而对精油微胶囊产品的品质及微观结构进行分析。结果表明,最佳的广佛手精油微胶囊制备工艺为:(1)壁材组合(阿拉伯胶:β-环糊精:麦芽糊精)的最佳配比为9:7:4 (g/g/g);(2)乳化工艺的最佳条件为:复合乳化剂配比(单甘酯:蔗糖脂肪酸酯)为3:7(g/g),用量为0.8%、芯材与壁材配比为3:7(g/g);(3)喷雾干燥的最佳条件为:进风温度180℃,雾化器频率30 Hz,进料流量55 mL/min。在此工艺条件下所制得的广佛手精油微胶囊具有较好的感官、物化特性及缓释性能,其包埋率高达85.32%,溶解度为93.25%,含水量低至2.65%,加热15 h挥发率只有12.24%,比未微胶囊化产品降低了79.47%。扫描电镜结果显示所制备的佛手精油微胶囊颗粒表面连续,呈较光滑的球形。因此,在最佳工艺条件下制备的广佛手精油微胶囊化产品具有良好的品质。
In this study, the preparation process of microcapsules using bergamot essential oil as the raw material was optimized, including wall material combination, emulsification process(emulsifier composition and dosage, core-to-wall material ratio) and spray drying conditions(inlet air temperature, atomizer frequency, feed flow rate). The optimal process parameters for microencapsulation of bergamot essential oil were first determined, and then the quality and microstructure of the resulting essential oil microcapsule products were analyzed. The results showed that the optimal conditions for preparing the bergamot essential oil microcapsules were:(1) The optimum ratio of wall material(arabic gum :β-cyclodextrin : maltodextrin) was 9:7:4(g:g:g);(2) The optimum conditions for emulsification included the ratio of composite emulsifier(monoglyceride : sucrose ester) as 3:7(g:g), a dosage of 0.8% for this composite emulsifier,and the core-to-wall material ratio as 3:7(g/g);(3)The optimized spray drying process was at an inlet air temperature of 180 ℃, atomizer frequency of 30 Hz, and feed flow rate of 55 mL/min.Under such optimal microcapsulation conditions, the obtained bergamot essential oil microcapsules possessed good sensory, physico-chemical and sustained release properties. The encapsulation rate and solubility of the products were as high as 85.32% and 93.25%, respectively, with the water content only at 2.65%. After being heated for 15 h, the products had only a volatilization rate of 12.24%, which was 79.47% lower than the unencapsulated products. The results of scanning electron microscopy showed that the obtained bergamot essential oil microcapsules were spherical in shape with smooth and continuous surfaces. Therefore, high-quality bergamot essential oil microcapsules could be produced under the optimized conditions.
In this study, the preparation process of microcapsules using bergamot essential oil as the raw material was optimized, including wall material combination, emulsification process(emulsifier composition and dosage, core-to-wall material ratio) and spray drying conditions(inlet air temperature, atomizer frequency, feed flow rate). The optimal process parameters for microencapsulation of bergamot essential oil were first determined, and then the quality and microstructure of the resulting essential oil microcapsule products were analyzed. The results showed that the optimal conditions for preparing the bergamot essential oil microcapsules were:(1) The optimum ratio of wall material(arabic gum :β-cyclodextrin : maltodextrin) was 9:7:4(g:g:g);(2) The optimum conditions for emulsification included the ratio of composite emulsifier(monoglyceride : sucrose ester) as 3:7(g:g), a dosage of 0.8% for this composite emulsifier,and the core-to-wall material ratio as 3:7(g/g);(3)The optimized spray drying process was at an inlet air temperature of 180 ℃, atomizer frequency of 30 Hz, and feed flow rate of 55 mL/min.Under such optimal microcapsulation conditions, the obtained bergamot essential oil microcapsules possessed good sensory, physico-chemical and sustained release properties. The encapsulation rate and solubility of the products were as high as 85.32% and 93.25%, respectively, with the water content only at 2.65%. After being heated for 15 h, the products had only a volatilization rate of 12.24%, which was 79.47% lower than the unencapsulated products. The results of scanning electron microscopy showed that the obtained bergamot essential oil microcapsules were spherical in shape with smooth and continuous surfaces. Therefore, high-quality bergamot essential oil microcapsules could be produced under the optimized conditions.
引文
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[14]郑义,俞益芹,黄陈,等.桂花精油微胶囊制备工艺优化[J].食品工业科技,2018,39(10):216-221ZHENG Yi,YU Yi-qin,HUANG Chen,et al.Optimum processing of osmanthus essential oil microcapsule[J].Science and Technology of Food Industry,2018,39(10):216-221
[15]刘双双,张彦军,徐飞,等.香草兰精油微胶囊的制备工艺优化及缓释性分析[J].热带作物学报,2018,39(7):1423-1430LIU Shuang-shuang,ZHANG Yan-jun,XU Fei,et al.Process optimization and slow release analysis of vanilla oil mi-croencapsulated[J].Chinese Journal of Tropical Crops,2018,39(7):1423-1430
[16]赵保堂,蔡苗苗,刘京,等.沙枣花精油微胶囊制备工艺优化及缓释性能[J].食品工业科技,2018,39(15):158-164ZHAO Bao-tang,CAI Miao-miao,LIU Jing,et al.Optimization of microencapsulation preparation process and controlled-release properties of Elaeagnus angustifolia flowers essential oil[J].Science and Technology of Food Industry,2018,39(15):158-164
[17]时慧,敬思群.茴香精油微胶囊制备工艺优化[J].中国酿造,2012,31(8):112-116SHI Hui,JING Si-qun.Optimization of preparation technology of fennel essential oil microcapsules[J].China Brewing,2012,31(8):112-116
[18]许杭琳.佛手精油的加工及综合利用技术的研发[D].金华:浙江师范大学,2013XU Hang-lin.Finger citron essential oil processing and comprehensive utilization techniques[D].Jinhua:Zhejiang Normal University,2013
[19]杨慧,周爱梅,夏旭,等.低温连续相变萃取广佛手精油及其组成分析[J].食品工业科技,2015,36(16):289-293YANG Hui,ZHOU Ai-mei,XIA Xu,et al.Study on the extract technology and component analysis of bergamot essential oil by low-temperature continuous phase transition[J].Science and Technology of Food Industry,2015,36(16):289-293
[20]王玉杰.单形格子和单形重心设计统计模型的优化分析方法[J].生物数学学报,1998,1:124-128WANG Yu-jie.The optimization method for statistical models in experiment designs of simplex lattice and simplex centre[J].Journal of Biomathematics,1998,1:124-128
[21]廖玉琴.柠檬果皮精油提取、微胶囊化工艺及抑菌性研究[D].成都:西华大学,2013LIAO Yu-qin.Study on extraction,microcapsule technology and antibacterial of lemon essential oil[D].Chengdu:Xihua University,2013
[22]赵巍,王军,段长青,等.喷雾干燥法制备微胶囊化山葡萄籽油粉末油脂[J].中国粮油学报,2009,24(12):77-83ZHAO Wei,WANG Jun,DUAN Chang-qing,et al.Manu facturing microcapsules of amur grape seed oil by spray-drying[J].Journal of the Chinese Cereals and Oils Association,2009,24(12):77-83
[23]张泳,赵力超,贺丽苹,等.低温连续相变制备酱油渣膳食纤维及其特性研究[J].现代食品科技,2014,30(5):185-190ZHANG Yong,ZHAO Li-chao,HE Li-ping,et al.Preparation and characterization of soy sauce residue dietary fiber using low temperature continuous phase transition extraction[J].Modern Food Science and Technology,2014,30(5):185-190
[24]万婷婷,罗爱平,张小永,等.乳化包埋法制备花椒精油微胶囊的研究[J].中国调味品,2011,36(2):34-39WAN Ting-ting,LUO Ai-ping,ZHANG Xiao-yong,et al.Preparation of micropsulation Zanthoxylum essential oil with emulsion inclusion method[J].China Condiment,2011,36(2):34-39
[25]杨军君,陈振林,陈光斌,等.红瓜子油微胶囊化的乳化工艺研究[J].食品工业,2018,39(2):47-50YANG Jun-jun,CHEN Zhen-lin,CHEN Guang-bin,et al.Study on emulsification technology of red melon seed oil microencapsulation[J].The Food Industry,2018,39(2):47-50
[26]胡建军,周冀衡,柴家荣,等.多指标正交试验数据的优化分析及应用[J].中国烟草学报,2008,14(2):9-14HU Jian-jun,ZHOU Ji-heng,CHAI Jia-rong,et al.Analysis and optimization of data from orthogonal experiments[J].Acta Tabacaria Sinica,2008,14(2):9-14
[27]李延辉.微胶囊化榛仁油的制备技术及工艺研究[D].长春:吉林农业大学,2005LI Yan-hui.Study on the technology of microencapsulated hazelnut oil[D].Changchun:Jilin Agricultural University,2005
[28]徐文秀,吴彩娥,李强,等.丁香油喷雾干燥微胶囊技术研究[J].食品科学,2006,1:278-281XU Wen-xiu,WU Cai-e,LI Qiang,et al.Study on processing technology of clove essential oil microencapsulation by spray-drying method[J].Food Science,2006,1:278-281
[2]赵秀玲.佛手生理活性成分的研究进展[J].食品工业科技,2012,33(21):393-399ZHAO Xiu-ling.Research progress of physiologically active compounds of bergamot[J].Science and Technology of Food Industry,2012,33(21):393-399
[3]钟艳梅,田庆龙,肖海文,等.不同产地佛手药材的化学成分比较研究[J].中南药学,2014,1:63-66ZHONG Yan-mei,TIAN Qing-long,XIAO Hai-wen,et al.Chemical constituents of fructus citri sarcodactylis from different places[J].Central South Pharmacy,2014,1:63-66
[4]魏玉君,邵邻相,麻艳芳,等.佛手叶挥发油的成分分析及生物活性研究[J].浙江师范大学学报(自然科学版),2014,3:329-333WEI Yu-jun,SHAO Lin-xiang,MA Yan-fang,et al.Study on constituents and biological activity of volatile oil from fingered citron leaves[J].Journal of Zhejiang Normal University(Nat.Sci.),2014,3:329-333
[5]Bagetta G,Morrone L A,Rombola L,et al.Neuropharmacology of the essential oil of bergamot[J].Fitoterapia,2010,81(6):453-461
[6]Peng C H,Ker Y B,Weng C F.Insulin secretagogue bioactivity of finger citron fruit(Citrus medica L.var.Sarcodactylis Hort,Rutaceae)[J].Journal of Agricultural&Food Chemistry,2009,57(19):8812-8819
[7]Saiyudthong S,Marsden C A.Acute effects of bergamot oil on anxiety-related behaviour and corticosterone level in rats[J].Phytotherapy Research,2011,25(6):858-862
[8]施长春,王建英,朱婉萍,等.佛手挥发油对哮喘的治疗作用[J].中华实用儿科临床杂志,2010,25(4):287-288SHI Chang-chun,WANG Jian-ying,ZHU Wan-ping,et al.Therapeutic effect of bergamots volatile oil on asthma[J].Chinese Journal of Applied Clinical Pediatrics,2010,25(4):287-288
[9]何云芳,金晓玲.佛手的研究现状及发展前景[J].经济林研究,2001,4:41-43HE Yun-fang,JIN Xiao-ling.Review of research progress in citrus medica with reference to prediction of development prospects[J].Economic Forest Researches,2001,4:41-43
[10]吕沛峰,高彦祥,毛立科,等.微胶囊技术及其在食品中的应用[J].中国食品添加剂,2017,12:166-174LYU Pei-feng,GAO Yan-xiang,MAO Li-ke,et al.Microencapsulation technology and its application in food[J].China Food Additives,2017,12:166-174
[11]张永清,贾燕冉,王德国.微胶囊技术及其在食品中的应用[J].许昌学院学报,2017,36(5):89-92ZHANG Yong-qing,JIA Yan-ran,WANG De-guo.Microcapsulating techniques and application in food[J].Journal of Xuchang University,2017,36(5):89-92
[12]王延圣,苏平.微胶囊技术在植物精油中的应用及研究进展[J].食品工业科技,2012,33(10):453-456WANG Yan-sheng,SU Ping.Application and research development of microencapsulation in plant essential oil[J].Science and Technology of Food Industry,2012,33(10):453-456
[13]王月月,段续,任广跃,等.洋葱精油微胶囊制备工艺优化及其品质分析[J].食品科学,2018,39(12):232-238WANG Yue-yue,DUAN Xu,REN Guang-yue,et al.Optimization of preparation technology and quality of onion essential oil microcapsules[J].Food Science,2018,39(12):232-238
[14]郑义,俞益芹,黄陈,等.桂花精油微胶囊制备工艺优化[J].食品工业科技,2018,39(10):216-221ZHENG Yi,YU Yi-qin,HUANG Chen,et al.Optimum processing of osmanthus essential oil microcapsule[J].Science and Technology of Food Industry,2018,39(10):216-221
[15]刘双双,张彦军,徐飞,等.香草兰精油微胶囊的制备工艺优化及缓释性分析[J].热带作物学报,2018,39(7):1423-1430LIU Shuang-shuang,ZHANG Yan-jun,XU Fei,et al.Process optimization and slow release analysis of vanilla oil mi-croencapsulated[J].Chinese Journal of Tropical Crops,2018,39(7):1423-1430
[16]赵保堂,蔡苗苗,刘京,等.沙枣花精油微胶囊制备工艺优化及缓释性能[J].食品工业科技,2018,39(15):158-164ZHAO Bao-tang,CAI Miao-miao,LIU Jing,et al.Optimization of microencapsulation preparation process and controlled-release properties of Elaeagnus angustifolia flowers essential oil[J].Science and Technology of Food Industry,2018,39(15):158-164
[17]时慧,敬思群.茴香精油微胶囊制备工艺优化[J].中国酿造,2012,31(8):112-116SHI Hui,JING Si-qun.Optimization of preparation technology of fennel essential oil microcapsules[J].China Brewing,2012,31(8):112-116
[18]许杭琳.佛手精油的加工及综合利用技术的研发[D].金华:浙江师范大学,2013XU Hang-lin.Finger citron essential oil processing and comprehensive utilization techniques[D].Jinhua:Zhejiang Normal University,2013
[19]杨慧,周爱梅,夏旭,等.低温连续相变萃取广佛手精油及其组成分析[J].食品工业科技,2015,36(16):289-293YANG Hui,ZHOU Ai-mei,XIA Xu,et al.Study on the extract technology and component analysis of bergamot essential oil by low-temperature continuous phase transition[J].Science and Technology of Food Industry,2015,36(16):289-293
[20]王玉杰.单形格子和单形重心设计统计模型的优化分析方法[J].生物数学学报,1998,1:124-128WANG Yu-jie.The optimization method for statistical models in experiment designs of simplex lattice and simplex centre[J].Journal of Biomathematics,1998,1:124-128
[21]廖玉琴.柠檬果皮精油提取、微胶囊化工艺及抑菌性研究[D].成都:西华大学,2013LIAO Yu-qin.Study on extraction,microcapsule technology and antibacterial of lemon essential oil[D].Chengdu:Xihua University,2013
[22]赵巍,王军,段长青,等.喷雾干燥法制备微胶囊化山葡萄籽油粉末油脂[J].中国粮油学报,2009,24(12):77-83ZHAO Wei,WANG Jun,DUAN Chang-qing,et al.Manu facturing microcapsules of amur grape seed oil by spray-drying[J].Journal of the Chinese Cereals and Oils Association,2009,24(12):77-83
[23]张泳,赵力超,贺丽苹,等.低温连续相变制备酱油渣膳食纤维及其特性研究[J].现代食品科技,2014,30(5):185-190ZHANG Yong,ZHAO Li-chao,HE Li-ping,et al.Preparation and characterization of soy sauce residue dietary fiber using low temperature continuous phase transition extraction[J].Modern Food Science and Technology,2014,30(5):185-190
[24]万婷婷,罗爱平,张小永,等.乳化包埋法制备花椒精油微胶囊的研究[J].中国调味品,2011,36(2):34-39WAN Ting-ting,LUO Ai-ping,ZHANG Xiao-yong,et al.Preparation of micropsulation Zanthoxylum essential oil with emulsion inclusion method[J].China Condiment,2011,36(2):34-39
[25]杨军君,陈振林,陈光斌,等.红瓜子油微胶囊化的乳化工艺研究[J].食品工业,2018,39(2):47-50YANG Jun-jun,CHEN Zhen-lin,CHEN Guang-bin,et al.Study on emulsification technology of red melon seed oil microencapsulation[J].The Food Industry,2018,39(2):47-50
[26]胡建军,周冀衡,柴家荣,等.多指标正交试验数据的优化分析及应用[J].中国烟草学报,2008,14(2):9-14HU Jian-jun,ZHOU Ji-heng,CHAI Jia-rong,et al.Analysis and optimization of data from orthogonal experiments[J].Acta Tabacaria Sinica,2008,14(2):9-14
[27]李延辉.微胶囊化榛仁油的制备技术及工艺研究[D].长春:吉林农业大学,2005LI Yan-hui.Study on the technology of microencapsulated hazelnut oil[D].Changchun:Jilin Agricultural University,2005
[28]徐文秀,吴彩娥,李强,等.丁香油喷雾干燥微胶囊技术研究[J].食品科学,2006,1:278-281XU Wen-xiu,WU Cai-e,LI Qiang,et al.Study on processing technology of clove essential oil microencapsulation by spray-drying method[J].Food Science,2006,1:278-281