采用热裂解-气相色谱/质谱(PY-GC/MS)联用技术研究了乙酸芳樟酯在350℃及900℃下的热裂解行为.结果表明:(1)不同的裂解温度直接影响生成产物的类型和相对含量;(2)乙酸芳樟酯可裂解生成41种物质,在350℃及900℃下,约有29.6%和41.3%的乙酸芳樟酯发生了热裂解;(3)随着裂解温度的升高,形成的危害性芳香烃类化合物(甲苯、对甲苯等)的相对含量有增加.根据乙酸芳樟酯裂解产物的种类和相对含量的变化,对其裂解产物的形成机理进行了探讨.
利用微波萃取技术,通过L9(34)正交试验设计优化工艺参数.结果表明,以85%乙醇为溶剂、提取温度55℃,微波功率150 W,每次提取15 min,提取2次,固液比1:7,提取率达26.84%.GC-MS分析表明五指山红茶提取物的挥发性成分有40种,这些成分具有不同香韵,赋予五指山红茶提取物丰富、纯正的蜜甜茶香.
为了更好地保留大蒜油的新鲜风味和有效成分,利用低温-微波提取技术,在配合添加干蒜粉下,于单因素试验的基础上,运用L9(34)正交试验设计研究了微波时间、微波功率、提取温度、固液比4个因素对大蒜油中硫含量的影响,获取新鲜大蒜油的微波提取最佳工艺参数.结果表明:当以辛癸酸甘油酯作溶剂、微波时间4 min、微波功率250 W、提取温度40℃、固液质量比1︰0.8时,获得的大蒜油中硫含量为质量分数0.4649%.
采用GC-MS法分析紫罗兰叶净油化学成分,共鉴定出45种化合物,其中 α-亚麻酸含量最高,相对质量分数达到46.402%,其次为棕榈酸,相对质量分数为14.693%.高级脂肪酸类物质相对质量分数之和达79.403%.另外,高级脂肪酸酯类物质的含量也较高,相对质量分数之和达17.84%.其余物质总计占到1.947%.紫罗兰叶净油卷烟加香的评吸结果显示,其可以明显增加青香、花香、甜香和膏香,赋予卷烟清香型风格特征,对提升烟气浓度和烟香丰富性,降低刺激、杂气,提高感官舒适度等效果显著.
通过Koenigs-Knorr糖苷化反应合成了柏木醇葡萄糖苷,对产物进行了表征,确认了化合物的结构,并对反应条件进行了优化,提高了收率.同时,对柏木醇葡萄糖苷的香气进行了评价,将其应用于卷烟中能明显改善烟气的状态及香气品质.
Glucose modification was proposed to modify activated carbons (ACs) to regulate bonding force between ACs and-phenylethanol. Effects of modification temperature on ACs pore structure and surface groups, and thus for their performances of adsorption and desorption -phenylethanol were investigated. Results show that glucose modification have no significant influence on absorbtion profermance of ACs. However, the modification increased acid sites on surface, which probably weakened π-π dispersion force between carbon surface and -phenylethanol. Because of that, desorption property of modified ACs was probably improved.
The chemical constituents of two kinds of clove bud oils obtained by supercritical CO2 extraction (SFE-CO2) and steam distillation were analyzed with GC - MS, their aroma and application in cigarettes were evaluated as well. Thirty - two and twenty - five components were identified in two oils, in which there were 12 common components. The aroma of oil obtained by SFE - CO2 was mainly spicy, fruity, and woody with slightly floral note, which formed its rich and strong aroma profile. While the aroma of oil obtained by steam distillation was mainly spicy and fruity, its aroma profile showed soft, clean and sweet tones. The appropriate amount of two kinds of oils in cigarette were 30 - 50 mg/kg. The SFE - CO2 obtained oil had the effect of enhancing and enriching smoking quality. Its unique aroma character made it showing a favorable effect in cigarette, so it could be used as a cigarette flavor according to practical requirements.
In order to compare the differences between aromatic components in cocoa powder and cocoa shell, and the differences between their application effects in cigarette, the roasted cocoa beans was prepared into tinctures, and their volatile aromatic components were identified by gas chromatography - mass spectrometry (GC - MS), and two kinds of tinctures were applied to cigarettes to compare their effects. Results showed that:①Thirty - eight and thirty - six kinds of aromatic components in the tinctures of cocoa and cocoa shell were identified respectively, including 29 kinds of same components, and the main components were obromine and caffeine. Nine kinds of unique components in cocoa tincture were identified, their aroma were milky, acid, roast and sweet; seven kinds of unique components in cocoa shell tincture were identified, their aroma were burnt, woody, nutty and roast;②The evaluation results showed that the best mass dosage of two tinctures in“coco palm” blank leaf were 0.3%. Cocoa powder tincture mainly provided cocoa characteristic aroma in cigarettes, while cocoa shell tincture mainly brought roast and nutty aroma. Therefore, two kinds of tinctures should be selected according to the requirements duringflavouring.
The method for determining the content of kaempferia-camphor in kaempferia essential oil by ultraviolet spectro-photometry was developed. The kaempferia-camphor was used as a standard substance and detected at its maximum absorption wavelength 309 nm,the linear standard curve was obtained with correlation coefficient of 0. 99991. This method was accurate,easy and economic with the average recovery of 99. 6%. It can be used for quantitative detection of target products.
以壳聚糖、三聚磷酸钠和海藻酸钠为壁材,油性物质为芯材,采用复凝聚技术制备微胶囊保润剂.结果表明:微胶囊保润剂的粒径为60 μm~200 μm,大部分呈规则球形,表面较圆整,为多核心颗粒微胶囊.温度大于200℃时微胶囊壁开始分解破裂释放芯材.与丙二醇相比,微胶囊保润剂具有更好的保润和防潮性能且感官评价效果较好.
The essential oils of clove bud from Indonesia,Madagascar,India and Vietnam were obtained by steam distillation, their extraction yields were 11 .07%,13.83%,13.32% and 12.04%,respectively.The main constituents of oils were ana-lyzed by GC-MS,the results showed that the total relative contents ofβ-caryophyllene,eugenol and eugenyl acetate in all vola-tile components of four oils were all over 90%,as 97.00% in Indonesia,93.74% in Madagascar,93.83% in India and 97.33% in Vietnam.Their odor profiles were compared and the cause of difference was discussed.
To prepare corn porous starch granule flavored with heat-sensitive mint oil microcapsule used for filter,the formu-lation and preparation technology were optimized,and its property was evaluated. The granule was prepared by extrusion-spheronization method,HPLC was used to determine release volatilization rate of mint oil,and HS-GC was used to determine mint oil encapsulation efficiency. The preparation processes of granule were optimized by single factor tests and orthogonal ex-periment methodL9(34). The optimized conditions were showed as follows(A3D3C1B2):mass ratio of corn porous starch to HPMC 200/1 ,orifice diameter 0.45 mm,screw speed 30 r/min,water dosage 25% . Under optimal conditions,the production rate of granule was (85.3±1)% ,release volatilization rate was (56.68±0.1)% ,comprehensive score was (68.14±1). Thermal analysis showed that the granule had a good release effect at low temperature,it was suitable for filter flavoring.
In this research,preparation process of mint oil nano-microemulsion was optimized by single factor test and orthogonal experiment.The optimized conditions were showed as follows: 30 ℃ constant temperature water bath,mint oil capacity 12%,emulsifier dosage 12%(T20 10%,P1570 2%),cosurfactants PG dosage 20%,PEG-400 dosage 5%,deionized water dosage 51%,shear emulsification speed 5 800 r/min.The physical and chemical characteristics of the microemulsion prepared were O/W microemulsion,particle size not more than 100 nm,relative density 1.0270,refractive index 1.3944,mint oil capacity(11.0±0.5)%,encapsulating rate 90% at 30 ℃,stable at 60 ℃.
Industrial microwave extraction technology is still in the exploratory stage, and design and improve- ment of large-scale equipment must depend on microwave extraction technology; pilot-scale experiments showed that: selecting the appropriate microwave effective exposure time, the microwave power and the solid-liquid ratio is conducive to energy conservation and efficiency; The extraction index (A) and energy consumption index (B) were obtained from the corresponding experimental data, and the experimental results show: when the ex- traction rates were greater than or equal to 95% , the energy consumption of dynamic microwave extraction is less than one of the solvent extraction 20% - 67%. Thus, relative to the solvent reflux extraction, microwave extraction is a new energy efficient technology; A new evaluation for large-scale microwave extraction equipment was shown by two indexes A and B at the same time.
Flavor compounds in fresh garlic oil are complex,but they are all sulfur-containing organic compounds.According to the fact,we established the new method first time to the determination of flavor compounds in the garlic oil——Microwave digestion barium sulfate turbidimetry.The experiments were designed to explore the amount of HNO3 for digestion garlic oil,the best measurement wavelength and the best measurement time.The conclusion is that when 0.300 garlic oil was measured,the amount of HNO3 was 1.3 mL,the best determination wave was 420 nm and the best determination time range was 5~50 min.Then a standard curve was drawn according to the results,the correlation coefficient R=0.99793,the content of flavor compounds in the garlic oil was 0.2871%.According to stability,reproducibility tests,the results are as followings: RSD separately is 1.69% and 0.669%,not more than 5%,the average recovery was 102.13%.The method is simple and convenient,with high accuracy and reliability,lower cost,applicability,suitable for corporate laboratories.
The kelp extract is nutrient-rich and natural flavor, which was made by microwave extraction in low-temperature. In this paper the drying method for the kelp extract was studied, including the single factor method and L9(3^4) orthogonal experimental design method, then the factors to effect removing the dried block from a plate was discussed. The main 4 factors to effect drying result are temperature, vacuum, the sample thickness and water content of the extract. Our experiments shows that the best drying conditions are drying temperature 90 %, vacuum 0.1 MPa, sample thickness of 1 cm, 16% moisture content before drying, and drying time of 50 min. Under the above condition, the drying process is simple and fast, average drying rate is 0.6056 g/min, moisture content of dried kelp extract is 5.82%, and the dried block is easily removed from the plate.
In the paper,the practice of reform of graduation thesis and culture of application research personnel is discussed.A new teaching mode is as follows: using the patent literature as the basic background information and proposed products as targeted research program,introducing the industry mentors to the students for raising their practical experience in laboratory experiment.In this way students talents in writing academic thesis and doing practical experiments are fully cultivated.
Study on the extraction and conditions of hesperidin in Pericarpium citri reticulatae under the detection of UV Absorption Spectrum.Experiment shows that hesperidin under certain conditions has a higher extraction rate and the higher purity:in the microwave irradiation,the petroleum ether-methanol-60% ethanol extraction in three steps,the third step in a 60% ethanol extract can be access to 80% of the hesperidin;UV detection under certain conditions may be to monitor and quantitative determination of hesperidin in the extract :The step-by-step,after extraction with petroleum ether and methanol and removal of interference,UV method will facilitate rapid determination of hesperidin content,the method is as:0.1% NaOH-75% ethanol is as blank and solvent,detecting under 362 nm,reference HPLC method,the results are with good accuracy;simplifying extraction process of hesperidin is as follows:extracted Pericarpium citri reticulatae three times by 95% ethanol under microwave irradiation,and then extracted the residue by 60% ethanol to get the result.
Sourced from wide and innovative patesns of EPO, USPTO and ISPO, selected food emulsifier industry, especially the famous companies in China, we investigated the intellectual property rights situation of the companies and compared them with the famous foreign ones, then analyzed the history, present status and tendency, found out the advantage and distance, finally put forward our suggestions to help the advanced companies choosing the derection and characteristics and to acceleate the industry develop.
Based on the static state-microwave extraction(SWE) in a small test by single factor tests, the dynamic-microwave extraction (DME) equipment was designed to extract black pepper oleoresin on pilot ex- periment scale. In the pilot experiment, the 4 parameters were chosen: microwave power, material flux, total solidliquid ratio and extraction times, the orthogonal experiments L9(34) were carried on to choose the best technics parameters and the results are as follows: 95% ethanol was as solvent, microwave power 2400 W, material flux 52 L/h, total solid-liquid ratio 1∶7 and extraction times 3. Under the above condition, the extraction rate of black pepper oleoresin is 12.69% and the piperine content for the raw material is 4.780% . In the paper, the 2 concepts of microwave effective time and microwave effective irradiation were put forward to explain the problems came from the transform process between SWE in the small test and DME in the pilot experiment.