浅谈三种茴香油及工业生产方法

文章主要介绍了三种茴香油(即大茴香油、茴香油、小茴香油)的性质和用途，深加工产品情况及工业生产方法。并详细阐述了工业生产上在常压下用水蒸气蒸馏法来制取大茴香油的工艺过程、主要设备和生产步骤。文章最后对该产品的经济效益和发展前景进行了分析。     

固相微萃取/气相色谱-质谱法分析小茴香挥发性成分

考察了萃取样品温度、萃取纤维吸附时间及解吸时间对于固相微萃取的影响,确定了固相微萃取小茴香挥发性成分较佳的实验条件为:萃取样品温度60℃,萃取纤维吸附时间40min,脱附温度250℃,脱附时间5min。用计算机谱库检索结合气相色谱保留指数二维定性方法,从小茴香的固相微萃取/气相色谱-质谱联用分析谱图中,鉴定出反式-茴香脑、顺式-茴香脑、爱草脑、葑酮、p-茴香醛、1,8-桉树脑、樟脑等35种小茴香挥发性成分,总质量分数98·70%。     

茴油臭氧化选择性的研究

研究了无水乙醇等溶剂对茴油臭氧化的影响以及茴油中三种主要双键物茴脑、α-蒎烯和草蒿脑臭氧化的选择性。研究结果表明 ,采用混合溶剂效果较好 ,混合溶剂的质量比为无水乙醇∶环己烷 =1∶ 3。臭氧对茴脑有很好的选择性     

茴香醛的合成研究进展

综述了合成茴香醛的研究进展情况,介绍了新技术在合成中的应用和发展趋势,着重对间接电氧化法氧化茴香脑制备茴香醛进行了评述。     

Methanol and Major Volatile Compounds of Turkish Raki and Effect of Distillate Source

Turkish Raki is the traditional anise flavoured distillate beverage produced mainly from a grape distillate called suma. Two types of Raki are produced in Turkey according to the distillate source. They are Type I — a fresh grape Raki produced only from suma and Type II — a Raki produced from a blended distillate of suma and alcohol of agricultural origin (mainly molasses). In this study the content of ethanol, methanol, distillate based major volatile compounds (aldehydes, esters, higher alcohols), aniseed based anethole and estragole, volatile acid and sugar values in two types of commercial Raki samples (40 samples) was determined and the effect of distillate source on the composition was examined. The distillate and the aniseed based major compounds of the Raki samples were analysed by direct injection with a GC‐MS‐FID according to the European Commission Reference Method. The results of variance analysis and PCA showed that there was a significant difference between the two types of Raki samples. Total volatiles (esters and higher alcohols), methanol, trans‐anethole, estragole and sugar values were higher in the samples made from suma alone. All of the analysed component levels of the Turkish Raki samples were in compliance with Turkish Distilled Beverage Regulations. The methanol levels ranged between 28.00–50.87 g/hL absolute alcohol (AA) in Type I samples and 22.03–41.06 g/hL AA in Type II samples. Distillate based total volatiles levels ranged between 136.12–147.88 g/hL AA, with a mean value of 142.88 g/hL AA, in Type I samples and 102.44–113.45 g/hL, with a mean value of 107.9 g/hL, in the Type II samples. The anise based compound trans‐anethole levels were significantly higher in the Type I samples (1,298–1,570 mg/L) than in the Type II samples (1,014–1,199 mg/L). According to distillate based volatiles, the Turkish Raki has a valuable content of volatile substances compared to other anise flavoured spirits.     

Extraction Kinetics and Anethole Content of Fennel (Foeniculum vulgare) and Anise Seed (Pimpinella anisum) Extracts Obtained by Soxhlet,Ultrasound, Percolation,Centrifugation, and Steam Distillation

Foeniculum vulgare (fennel) and Pimpinella anisum (anise) extracts were obtained by Soxhlet, cold percolation, ultrasound assisted extraction, and centrifugal extraction using ethanol as solvent; anise extracts were also obtained by steam distillation. Soxhlet presented the highest yields for both fennel and anise seed (16.8% and 23.3%, respectively). The highest anethole content among ethanolic extracts was obtained for centrifugal extraction (6.8 mg/g and 143 mg/g for fennel and anise extracts, respectively). Steam distillation presented low yield (0.26%), but high anethole content (68–98%, area). Anise ethanolic extracts also tested positive for flavonoids.     

高纯度天然大茴香脑生产技术研究

以八角茴香油为原料,采用静态冷冻工艺冷冻、离心制备得到粗产品,再采用网波不锈钢填料分馏塔对粗产品进行精馏分离得到高纯度大茴香脑（纯度〉99％）。产品按国家标准GB23489—2（）（19的要求进行检验。此工艺路线简单、实用,产品品质优良．是生产高纯度天然大茴香脑的新型实用方法。     

反式茴脑低温氧气氧化性质及其产物研究

考察了反式茴脑氧化反应特性,采用自行设计的小型密闭压力容器跟踪反应压力变化,利用碘量法分析了过氧化物浓度,利用气相色谱-质谱联用仪分析了反应产物种类。实验结果表明,压力变化显示,反式茴脑氧化过程分3个阶段:首先是缓慢吸收氧气阶段;然后是快速氧化反应阶段;最后是氧化趋于结束阶段。当反应温度为95℃,反应时间为4 h时,过氧化物浓度最大为85.07 mmol/kg;反式茴脑氧化反应产物比较复杂,最主要的产物有茴香醛、乙醛、茴香环氧化物、茴香二醇、茴香偶酰等,当反应温度为55℃时,茴香醛选择性达到70.36%。     

茴香脑间接电化学氧化合成茴香醛的研究

研究了以茴香脑为原料,用Ce4 /Ce3 作为氧化还原媒质,间接电化学氧化合成茴香醛。用正交实验和单因素实验分别研究了Ce4 氧化茴香脑合成茴香醛的化学氧化过程中各实验条件对产率的影响,并优化出了最佳反应条件:n(Ce4 )∶n(茴香脑)=2∶1,反应温度为30°C,硫酸浓度为0.5 mol/L,苯为溶剂。在优化条件下茴香醛产率达90%。     

单一羰基溶剂体系的茴脑臭氧化反应

以茴脑为原料,臭氧化法制备茴香醛。通过实验筛选出茴香醛产率较好的含羰基单一溶剂体系,并考察了溶剂种类、溶剂用量、臭氧流量和反应时间对反应结果的影响。优化的工艺条件为:乙酸乙酯或丙酮为溶剂,m(茴脑)∶m(溶剂)=1∶3,臭氧流量0.06 m3/h,反应时间80 min,在该条件下,茴脑转化率达100%,乙酸乙酯溶剂中茴香醛产率可达73.61%,丙酮溶剂中茴香醛产率可达74.54%。