栀子蓝色素的分步制备工艺

优化栀子蓝色素分步制备的工艺。以栀子黄生产废液提取物——京尼平苷为底物原料,以黑曲霉发酵制备的β-葡萄糖苷酶为转色酶,研究京尼平苷水解制备京尼平的影响因素,通过正交设计试验优化其工艺条件。以显色生成亮丽栀子蓝色素为目标,筛选显色氨基酸,制备色泽明亮的栀子蓝色素。结果表明,在添加8%粗β-葡萄糖苷酶量,反应温度55℃,p H 4.2,水解时间7 h条件下,京尼平产量最高;甲硫氨酸、甘氨酸、赖氨酸、丙氨酸等多种氨基酸均与京尼平反应生成蓝色素,其中甲硫氨酸显色反应生成物色泽亮丽,是由栀子蓝色素制备的适宜氨基酸;n_(甲硫氨酸)∶n_(京尼平苷)=6∶1、p H 7.0、显色温度80℃、时间10 h时,获得色泽明亮的栀子蓝色素,其色价为20.6。     

京尼平甙水解物与谷氨酸钠反应生成栀子蓝色素最佳条件的研究

对京尼平甙水解产物与谷氨酸钠反应生成栀子蓝色素的最佳条件进行了研究。结果表明,反应的最适温度为80℃,最适pH为7.5,当栀子黄废液的固形物含量为1%时,水解产物与0.7%的谷氨酸钠完全反应。     

京尼平甙水解物与谷氨酸钠反应生成栀子蓝色素最佳条件的研究

对京尼平甙水解产物与谷氨酸钠反应生成栀子蓝色素的最佳条件进行了研究。结果表明,反应的最适温度为80℃,最适pH为7.5,当栀子黄废液的固形物含量为1%时,水解产物与0.7%的谷氨酸钠完全反应。      

双发色结构栀子蓝染料的合成

以京尼平和赖氨酸为原料合成双发色结构的栀子蓝染料,探讨n(京尼平):n(赖氨酸)、温度和pH对反应的影响.结果表明:在n(京尼平):n(赖氨酸)=2:1、反应温度为80℃、pH为7的条件下,染料合成效率最高.用大孔吸附树脂对产物进行分离、纯化,经高效液相色谱法(HPLC)测定,具有很好的分离提纯效果.反应产物经红外和液...     

栀子蓝色素制备及纯化工艺的研究

本文采用纤维素酶水解京尼平甙生成京尼平,京尼平再与氨基酸合成栀子蓝色素,利用超滤技术对其进行分离、纯化.通过一系列的单因素实验和正交实验,探讨了制备及纯化栀子蓝色素的工艺条件.结果表明,最佳工艺条件为以谷氨酸钠作为氨基酸来源,液固比(V/m)=8:1,酶解时间6h,纤维素酶与京尼平甙的质量比1:8,氨基酸与京尼平甙的质量比1:2,反应时间96 h.最佳超滤纯化工艺为超滤膜截至分子量为5000 Da,超滤压力0.5～0.8 MPa,pH 7,超滤温度为室温.经HPLC测定,经本工艺制备的栀子蓝色素色价E590nm1cm(1%)≥192,纯度≥95%.     

京尼平与皮胶原的反应性研究

以从栀子属植物的果实中提取的环烯醚萜类化合物京尼平为代表,研究其与皮胶原的反应性。采用UV、TLC等方法并结合已有的文献资料,探讨了京尼平与皮胶原的反应机理。用DSC法分析了京尼平的鞣制效果,并对最佳鞣制条件(京尼平的用量、鞣制时间、鞣液温度及pH值等)进行了筛选。结果表明:用干皮粉质量5%的京尼平,在pH=7·5左右鞣制24h后,其DSC曲线的Tp可达到85℃,同时皮粉被染成深蓝色。因此我们认为,京尼平可以作为皮革工业的一种潜在的、可再生的、清洁高效的鞣剂和染料。     

栀子紫色素制备及其稳定性研究

利用纤维素酶水解京尼平苷后与氨基酸反应制备栀子紫色素。研究了栀子紫色素的光稳定性、热稳定性、pH稳定性和耐氧化还原性,并就食品中常见的金属离子和食品添加剂对栀子紫色素稳定性的影响进行探讨。结果表明:光照对栀子紫色素影响较小,在光照中,栀子紫色素呈微弱褪色趋势;栀子紫色素在80℃内比较稳定,随着时间的延长色素吸光度值呈微弱下降趋势,而在100℃中有较大褪色趋势;pH对栀子紫色素影响较大,在pH为6.0时吸光度值最高,因此栀子紫色素最好保存于弱酸性环境中;其抗氧化性较差,但对还原剂的耐受性良好;栀子紫色素不受大多数金属离子的影响,而在Zn2+、Fe2+、Fe3+与Cu2+环境中容易形成沉淀。大部分食品添加剂对栀子紫色素稳定性影响不大。栀子紫色素具有良好的理化性质,为栀子紫色素的生产应用提供了参考数据。     

京尼平和栀子黄对大豆蛋白纤维的染色研究

以开发用于再生蛋白质纤维染色的天然染料为出发点,采用京尼平和栀子黄对大豆蛋白纤维进行染色试验。研究两种染料的染色性能,确定最佳染色工艺条件,并对染色织物色牢度及抗菌性进行测试评价。结果表明：京尼平和栀子黄染色大豆蛋白纤维可获得较好的染色深度,两者对大豆蛋白纤维染色条件、染色牢度及抗菌性区别较大,栀子黄染色最佳条件为染料用量7%、pH值为5.0、染色温度80℃、染色时间1.0 h;京尼平染色最佳条件为染料用量5%、染色温度为35～40℃、pH值为7.5～8.5、染色时间2.0 h。京尼平染色牢度好于栀子黄,除了栀子黄的耐日晒色牢度稍差,其余各项色牢度均达到3级及以上。染色后的纤维抗菌性能良好,具有一定的使用价值。     

京尼平改性明胶在制革中的潜在应用

京尼平是一种从栀子果实中提取出来的环烯醚萜类化合物.由于其细胞毒性较低,京尼平常用来替代戊二醛和甲醛,作为交联剂使用.本文对京尼平改性明胶产品作为皮革填充剂使用进行了研究.首先优选了京尼平改性明胶的最佳反应条件.然后,按比例进行放大生产,制备出京尼平改性的明胶产品,并用其对蓝湿革的不同部位进行处理,再分别进行复鞣、染色和加脂,得到RCF坯革,然后测定成革的物理力学性能,并进行主观评价.结果表明,京尼平改性明胶产品处理后的坯革,物理力学性能与对照样相差不大,但感官性能(手感、丰满性、粒面褶纹和颜色)比对照样好得多.对蓝湿革和RCF坯革的湿热稳定性研究结果表明,RCF坯革的收缩温度高一些.扫描电子显微镜检测结果表明,皮革纤维明显地被京尼平改性明胶产品所包覆,这种现象在转谷氨酰胺酶改性明胶的研究中也曾发现.因此.京尼平改性明胶在制革过程中具有应用潜力,可以为传统的鞣后加工处理提供一种环境友好的替代产品.     

碱水解栀子苷大孔树脂分离纯化京尼平苷酸

目的:研究NaOH水解栀子苷,大孔树脂分离纯化京尼平苷酸的工艺。方法:用NaOH将栀子苷水解制备京尼平苷酸,并通过高效液相色谱法监测栀子苷的水解过程;比较7种大孔吸附树脂对京尼平苷酸的静态吸附和解析性能,筛选出一种吸附和解析性能较好的树脂,用动态柱层析法对京尼平苷酸进行分离纯化。结果:H103大孔树脂对京尼平苷酸的吸附和解析性能较好,动态吸附上样后用蒸馏水冲洗2 BV,再用30%乙醇洗脱2 BV,洗脱率达到95.2%,洗脱液真空干燥得到灰白色粉末,HPLC检测其纯度达96.1%。结论:采用碱水解栀子苷再用大孔树脂分离纯化京尼平苷酸,该工艺具有步骤少、收率高等优点,为京尼平苷酸的制备提供了一种新途径。     

基于化学修饰法制备油溶性栀子蓝色素及其性能表征研究

主要采用化学修饰法制备油溶性栀子蓝色素,对其制备工艺条件进行优化并评价其性能表征。采用硬脂酰氯对栀子蓝色素分子结构进行化学修饰,利用单因素逐级试验优化工艺条件,经SEM、FTIR及紫外-可见分光光度法对目标产物进行结构表征,并评价油溶性栀子蓝色素在不同条件下的溶解性和稳定性。结果表明,制备最佳工艺条件为反应物摩尔比n_{水溶性栀子蓝色素}∶n_硬脂酰氯∶n_三乙胺为1∶5∶5,反应温度为40℃,反应时间为30 h,在此条件下目标产物产量为(402±8.2)mg,色价为26.3±0.6;紫外-可见光谱图显示油溶性栀子蓝色素的最大吸收波长为624 nm;观察微观形貌发现化学改性前后栀子蓝色素微粒呈现明显不同的微观结构;FTIR分析显示目标产物在2919.98 cm^-1和2851.17 cm^-1处出现极强的吸收峰,而C-O、C-O-C-O和C-C的特征吸收峰明显降低,表明经化学改性发生了酯化反应,引入了脂肪酸长链和酯基等疏水性基团;栀子蓝色素衍生物可溶于丙酮,易溶于乙酸乙酯、石油醚和食用油等溶剂;制得的油溶性栀子蓝色素在室内散射光强度、阴暗避光条件及低温条件下稳定性良好。该研究得到一种油溶性栀子蓝色素的最佳工艺条件,一定程度上扩大了栀子蓝色素在食品中的应用范围。     

基于化学修饰法制备油溶性栀子蓝色素及其性能表征研究

主要采用化学修饰法制备油溶性栀子蓝色素,对其制备工艺条件进行优化并评价其性能表征。采用硬脂酰氯对栀子蓝色素分子结构进行化学修饰,利用单因素逐级试验优化工艺条件,经SEM、FTIR及紫外-可见分光光度法对目标产物进行结构表征,并评价油溶性栀子蓝色素在不同条件下的溶解性和稳定性。结果表明,制备最佳工艺条件为反应物摩尔比n_{水溶性栀子蓝色素}∶n_硬脂酰氯∶n_三乙胺为1∶5∶5,反应温度为40℃,反应时间为30 h,在此条件下目标产物产量为(402±8.2)mg,色价为26.3±0.6;紫外-可见光谱图显示油溶性栀子蓝色素的最大吸收波长为624 nm;观察微观形貌发现化学改性前后栀子蓝色素微粒呈现明显不同的微观结构;FTIR分析显示目标产物在2919.98 cm^-1和2851.17 cm^-1处出现极强的吸收峰,而C-O、C-O-C-O和C-C的特征吸收峰明显降低,表明经化学改性发生了酯化反应,引入了脂肪酸长链和酯基等疏水性基团;栀子蓝色素衍生物可溶于丙酮,易溶于乙酸乙酯、石油醚和食用油等溶剂;制得的油溶性栀子蓝色素在室内散射光强度、阴暗避光条件及低温条件下稳定性良好。该研究得到一种油溶性栀子蓝色素的最佳工艺条件,一定程度上扩大了栀子蓝色素在食品中的应用范围。     

响应面法优化栀子黄废液制备栀子蓝色素酶解工艺的研究

本实验以栀子黄浓缩废液为原料,栀子蓝色素色价为指标,通过酶种类、酶解时间、酶添加量、酶解pH单因素及响应面优化实验,制备高色价栀子蓝色素。实验结果表明:酶解栀子黄浓缩废液最适酶为纤维素酶,酶解pH为5.2,酶添加量为2.0%,酶解时间6.5 h,酶解温度55℃。在此酶解工艺条件下,酶解液中加入1%的组氨酸,80℃水浴5h,烘干后栀子蓝色素色价可达33.6。该工艺操作简单、成本低、栀子蓝色价高,可广泛应用于实际生产过程中。     

Determination of methanol in gardenia red and gardenia blue

The natural food color gardenia red is manufactured through the hydrolysis of the methyl ester of iridoid glucoside. Gardenia blue is also made from iridoid glucoside. Therefore, there is a possibility that the commercial products contain methanol. To determine methanol in gardenia red and gardenia blue, a headspace GC method with standard addition was developed. In the case of gardenia blue with the methyl ester, methanol may be formed during the analytical procedures for methanol. Thus, conditions in which methanol would not be produced in the headspace-GC method were investigated. Vials containing 1 g of the color preparation, 1 mL of water, and a standard solution were sealed. Equilibrium temperature was an important factor among the conditions for analyzing methanol in gardenia blue. Although at room temperature and 50 degrees C, the contents of methanol were equal, the content increased 1.2 times at 80 degrees C. Methanol contents determined at 50 degrees C were 8 and 9 micrograms/g in two gardenia red products and 25-34 micrograms/g in three gardenia blue products, which were below the residual limit of 50 micrograms/g set for many other natural food additives.     

Milk colloidal system as a reaction medium and carrier for the natural blue colorant obtained from the cross-linking between genipin and milk proteins

A promising natural blue colorant was obtained from the cross-linking between genipin and milk proteins. Milk was simultaneously used to extract genipin from the unripe genipap (Genipa americana L.) and evaluated as a reaction medium and carrier for the novel blue colorant. The effects of the milk composition (skimmed, semi-skimmed, and whole) on the kinetic of blue color formation in the colorant-loaded milk samples during their cold storage time for 96 h were evaluated using their color parameters and free-genipin content. The reaction between milk proteins and genipin were evaluated by FTIR spectroscopy. In addition, the blue colorant-loaded milk samples were characterized according to their droplet size distribution, microstructure, and phase separation kinetics. The milk fat content influenced the genipin recovery while the milk with higher protein content contributed to obtaining a more intense blue color. Using whole milk with 3.0 g/100 g fat content favored the light scattering and, thus, a blue colorant with a more intense −b¹ and L¹ values was obtained. On the other hand, the use of skimmed milk with 0.5 g/100 g fat content resulted in more consumption of genipin due to its more protein content for the reaction of blue color compounds formation. Thus, a more intense and darker blue coloration was observed with lower light scattering. The milk composition did not modify the phase separation kinetics of the blue colorant-loaded milk. Therefore, our results have demonstrated that the milk was a suitable medium for the reaction of blue color formation and also a good blue compounds carrier.Industrial relevanceConsumer demands for natural colorants have increased in the last years.Thus, the new food industry challenge is to develop novel healthy, safe and high-quality food products based on natural colorants. Currently, the colorant market does not have still available a natural blue colorant. Therefore, the development of a novel natural blue colorant from plant material could meet this worldwide demand increasing the added value of many products such as ice cream, dairy beverages, and candies.     

利用双水相萃取栀子黄废液中的栀子苷酶法生产栀子蓝色素的研究

研究有机溶剂/ 磷酸氢二钾双水相体系对栀子黄废液中栀子苷的萃取条件,并将萃取后的栀子苷用于栀子蓝色素的生产。根据分相后上下相中栀子苷的分配系数及两相体积比,选择合适的双水相体系,并改变溶剂与废液的体积比、磷酸氢二钾加入量、废液pH 值以及萃取温度等参数,研究萃取栀子苷的最佳条件。实验结果表明,乙醇/ 磷酸氢二钾为合适的萃取体系。当双水相体系总量为10ml 时,乙醇与栀子黄废液的体积比为6:4,加入磷酸氢二钾1.0g,体系分相完全后栀子苷分配系数(K)为4.56,两相体积比(R)为6.38,栀子黄废液pH 值及萃取温度在正常条件下对K 值及R 值影响不大。放大实验表明,以乙醇/ 磷酸氢二钾体系萃取栀子黄废液中的栀子苷,所得栀子苷纯度可达62.12%,收率可达96.32%。萃取后的栀子苷经β- 葡萄糖苷酶水解精氨酸显色后得到栀子蓝色素,色价E1% (590nm)65.92。     

Heat and light stability of three natural blue colorants for use in confectionery and beverages

The stabilities of three natural blue colorants—gardenia blue, phycocyanin and indigo—toward heat and light were studied in simple solutions of various pH. Gardenia blue was found to be stable at temperatures up to 80 °C in aqueous solution at pH 3, 5 and 7. Exposure to light of 3×10⁵ lux for 24 hours resulted in approximately 50% degradation of gardenia blue in aqueous solution. Phycocyanin was found to be unstable to heat and light in aqueous solution. Phycocyanin is insoluble in acidic solution (pH 3) and denatures at temperatures above 45 °C at pH 5 and 7, leading to a color change. Exposure to light of 3×10⁵ lux for 24 hours in aqueous solution at pH 5 and 7 caused ~80% degradation. Indigo was found to be stable in medium-chain-triglyceride oil for temperatures up to 90 °C, but to photodegrade (by approximately 70% after five hours of exposure to 3×10⁵ lux), corresponding to a quantum yield of 1.8×10^–4 mol Einstein^–1 for visible light and 1.4×10^–2 mol Einstein^–1 for UV, as determined for monochromatic light of 600 and 313 nm, respectively. Exploratory studies have been carried out with the three blue colorants in application media such as soft drink, jelly gum, hard candy and sugar coating for soft candy. Despite its lower stability towards heat and light, phycocyanin was concluded to be the more versatile blue food colorant among the three studied, showing a bright blue color in jelly gum and coated soft candy.     

栀子黄A238nm/A440nm 值与西红花苷和栀子苷相关性研究

目的：采用TLC、HPLC 和紫外分光光度法(UV)研究栀子黄OD 值(栀子黄中栀子苷的最大吸光度A238nm 与西红花苷的最大吸光度A440nm 的比值)与栀子苷含量的关系。方法：采用硅胶柱层析从栀子中分离西红花苷纯品,然后分别采用TLC、HPLC 和UV 来定性和定量分析栀子乙醇提取部位和经大孔吸附树脂精制的栀子黄,并计算波长238nm 和440nm 处的百分比吸光系数及OD 值。结果：经过对以上数据的分析,发现西红花苷本身在波长238nm处有明显紫外吸收,采用OD 值来控制栀子黄中的栀子苷将高估栀子苷含量。结论：栀子黄中栀子苷的控制不宜采用OD 值作为评价指标,而应采用具有分离功能的高效液相色谱法来作为质量控制的手段。     

蚕丝织物的栀子蓝色素染色

为解决蚕丝织物的天然染料染色缺少蓝色的问题,丰富天然染料染色蚕丝织物的色谱,用栀子蓝色素对蚕丝织物染色,研究了染色工艺对上染百分率的影响,依据栀子蓝色素上染蚕丝织物的上染速率曲线及吸附等温线分别研究了其染色动力学和染色热力学。得到栀子蓝色素上染蚕丝织物的最佳工艺为:染色pH值3,染色时间50 min,染色温度60 ℃。在60 ℃,pH值为3条件下染色,染色吸附过程符合准二级动力学模型,为化学吸附,吸附等温线为朗缪尔型,为定位吸附。据此计算,得到栀子蓝色素上染蚕丝织物的染色饱和值为 97.465 9 g/kg。     

维生素E对β-胡萝卜素纳米乳液性质及其饮料稳定性的影响

为提高β-胡萝卜素的水溶性和稳定性,本研究以吐温80、吐温60和磷脂为乳化剂,维生素E为抗氧化剂制备了纳米乳液.测定了纳米乳液的粒径、透光率、色价、储藏稳定性和应用稳定性.结果显示,维生素E对纳米乳液粒径和透光率有轻微影响,对包埋率和色价没有影响.在25、37℃和光照下储藏28 d期间纳米乳液的透光率没有发现明显变化,...