姜黄素的合成ppt课件
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姜黄色素生产工艺文本及流程图一、姜黄色素生产工艺说明:将原料姜黄首先经过筛分,去除石块杂土等机械杂质,再粉碎后投放到提取罐中提取,向提取罐中投入90%的乙醇,高温提取2h ,重复两次,合并两次提取液,回收乙醇进行浓缩,浓缩液加入乙酸乙酯萃取,重复5-6次,合并萃取液,回收乙酸乙酯,浓缩至一定比重得到的姜黄油树脂进入结晶桶,自然结晶,精致48h 以后进行离心分离,分离的姜黄素用乙醇充分洗涤,洗涤后的姜黄素进行真空干燥,干燥后的姜黄素进行粉粹过80目筛,最后检验合格后包装储存。
二、生产工艺流程图:乙醇提取 过滤 合并提取筛分 浓缩萃取分离浓缩粉粹过筛 检验药渣 结晶干燥姜黄 包装储存Curcumin production process flow chart1 Turmeric production process description:The raw material turmeric is first sieved to remove mechanical impurities such as rock and other soils, then crushed and then put into the extraction tank to extract 90% ethanol into the extraction tank, 2h at high temperature, repeat twice, merge the two extracts , The ethanol was concentrated, the concentrated solution was extracted with ethyl acetate, and the mixture was extracted for 5-6 times. The extract was combined and the ethyl acetate was recovered. The turmeric oil was concentrated to a certain proportion. The natural crystal was crystallized and refined after 48h Separation, separation of curcumin with ethanol to wash, washed curcumin after vacuum drying, dried curcumin powder over 80 mesh sieve, the final inspection after passing the packaging.2,Production flow chart:Turmeric raw materials →Screening separation→Ethyl alcohol extraction→filter→Merge extraction→concentrate → f urther↓Dregsextraction→Separation→concentrate→crystallization→dry →Powder sieving→test→Packaging and storage。
·实验研究·天然姜黄素类化合物的合成国大亮1,李艳梅2,朱晓薇1,张艳军1(1.天津中医药大学,天津300193;2.舒泰神(北京)生物制药股份有限公司,北京100176)摘要:目的以化学合成法制备天然姜黄素类化合物。
方法以对羟基苯甲醛或香草醛和乙酰丙酮为原料经硼络合保护,分别合成姜黄素、一脱甲氧基姜黄素和二脱甲氧基姜黄素,测定熔点,并以氢谱进行结构解析。
结果姜黄素、一脱甲氧基姜黄素和二脱甲氧基姜黄素合成品分别为亮黄色、橙黄色和橙红色粉末,氢谱所确证的结构与已知结构一致。
结论本合成法操作简单,条件温和,可在短时间内制备大量天然姜黄素类化合物,效率较传统的提取分离法大大提高。
关键词:天然姜黄素类化合物;姜黄素;一脱甲氧基姜黄素;二脱甲氧基姜黄素;合成中图分类号:R284.3文献标识码:A文章编号:2095-5375(2013)03-0125-003Synthesis of natural curcuminsGUO Da-liang1,LI Yan-mei2,ZHU Xiao-wei1,ZHANG Yan-jun1(1.Tianjin University of Traditional Chinese Medicine,Tianjin300193,China;2.Staidson BeijingBiopharmaceuticals Co.,Ltd.,Beijing100176,China)Abstract:Objective To prepare natural curcumins by chemical synthesis.Methods Curcumin,demethoxycurcum-min and bisdemethoxycurcumin were synthesized using p-hydroxybenzaldehyde or vanillin,together with acetylacetone by boron protection.Melting point and1H-NMR were determined to resolve the structures.Results Curcumin,demethoxy-curcummin and bisdemethoxycurcumin were bright yellow,orange and orange red powders.Structures were proved same as natural curcumins by melting points and1H-NMR.Conclusion This method was simple and easy to control.Amount of curcumins could be prepared in a short time.So it was more effective than traditional extraction methods in preparation of curcumins.Key words:Natural curcumins;Curcumin;Demethoxycurcumin;Bisdemethoxycurcumin;Synthesis姜黄素类化合物为姜黄属植物中的主要活性成分,具有预防和治疗癌症及脑神经保护等多种作用[1,2]。
食品安全国家标准食品添加剂姜黄素1 范围本标准适用于以姜科植物姜黄(Curcuma longa L.)的根茎为原料,经有机溶剂提取,再经物理方法精制而得的食品添加剂姜黄素。
2 化学名称、分子式、结构式和相对分子质量2.1 化学名称姜黄素:1,7-双(4-羟基-3-甲氧基苯基)-1,6-二烯-3,5-庚二酮脱甲氧基姜黄素:1-(4-羟基苯基)-7-(4-羟基-3-甲氧基苯基)-1,6-二烯-3,5-庚二酮双脱甲氧基姜黄素:1,7-双(4-羟基苯基)-1,6-二烯-3,5-庚二酮2.2 分子式:姜黄素:C21H20O6;脱甲氧基姜黄素:C20H18O5;双脱甲氧基姜黄素:C19H16O42.3 结构式:姜黄素:R1=R2=OCH3;脱甲氧基姜黄素:R1=OCH3,R2=H;双脱甲氧基姜黄素:R1=R2=H2.4 相对分子质量姜黄素:368.39(按2007年国际相对原子质量)脱甲氧基姜黄素:338.39(按2007年国际相对原子质量)双脱甲氧基姜黄素:308.39(按2007年国际相对原子质量)3 技术要求3.1 感官要求:应符合表1 的规定。
表1 感官要求3.2理化指标:应符合表2的规定。
表2 理化指标附录 A检验方法A.1 一般规定本标准所用试剂和水在没有注明其它要求时,均指分析纯试剂和GB/T6682-2008中规定的三级水。
试验中所用杂质测定用标准溶液、试剂溶液及样品溶液,在没有注明其它要求时,均按GB/T 601、GB/T 602和GB/T 603的规定制备。
A.2 鉴别试验A.2.1 试剂和材料A.2.1.1乙醚。
A.2.1.2冰乙酸。
A.2.1.3氢氧化钠溶液: 0.05 mol/L。
A.2.1.4盐酸: 1 mol/L。
A.2.1.5乙醇:95%。
A.2.1.6硫酸。
A.2.1.7硅胶薄层板:称取硅胶10 g,加水20 mL,置于研钵中研磨成稀稠适宜的浆状液,均匀涂布于玻璃板上,涂层厚为0.5 mm。