CN101225052A - Process for extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude product from red pepper - Google Patents

Process for extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude product from red pepper Download PDF

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CN101225052A
CN101225052A CN 200710300024 CN200710300024A CN101225052A CN 101225052 A CN101225052 A CN 101225052A CN 200710300024 CN200710300024 CN 200710300024 CN 200710300024 A CN200710300024 A CN 200710300024A CN 101225052 A CN101225052 A CN 101225052A
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capsicum
capsaicin
extraction
extract
pepper
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CN 200710300024
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CN101225052B (en )
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王海棠
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王海棠
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Abstract

The invention provides a technological method of extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude products from red pepper, which adopts the red pepper pulverized with a certain particle size as material and hydrous ethanol as extraction solvent, and three-stage extraction method for the preparation of the three extracts of capsaicin, capsicum oleoresin and capsicum red pigment separated in the extraction phase. The three extracts are respectively vacuum concentrated and distilled, and the crude products of capsaicin, capsicum red pigment and capsicum oleoresin can be gotten after the solvent recovery and solvent residue removal. The extracting and separating method separates the capsaicin, capsicum oleoresin and capsicum red pigment in the extraction phase by using the same extraction tank and solvent, avoids the trouble of separating the capsaicin and capsicum red pigment in the late workshop section, eliminates the alkali and acidification treatments or the separation craft of column chromatography, facilitates the improvement of the output ratio of capsicum red pigment and capsaicin. The technological method of extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude products from red pepper has the advantages of simple technique, easy operation and control, less equipment investment, easy solvent recovery and reuse, low cost, short cycle, high yield of active ingredient, and better suitability for commercial and mass production.

Description

从红辣椒中提取分离辣椒碱、辣椒红色素和辣椒精粗产品的工艺方法技术领域本发明属于精细化工生产行业领域,提出一种从红辣椒中提取分离辣椒碱、 辣椒红色素和辣椒精禾且产品的工艺方法。 Isolated from red pepper extract capsaicin The process of capsanthin and pepper Technical Field The present invention belongs to the forage to concentrate products produced fine chemical industries, to provide a paprika extract isolated from capsaicin, capsanthin and Capsicum Wo and the process for the product. 背景技术辣椒碱、辣椒精和辣椒红色素均有广泛和重要用途。 Background of the Invention Capsaicin, Paprika Oleoresin Capsicum and have extensive and important uses. 辣椒te要用于医药、生化农药、功能涂料和防卫雌4个方面。 Pepper te to be used in the pharmaceutical, biochemical pesticides, functional coatings and defense female four aspects. 辣椒红色素主要用作食品添加剂, 可使多种食品以多种色调着色;广泛用于医药、化妆品和鸡鸭等禽类高级饲料生产中;国外已大量用于纺织品染色,以及涂料、塑料的着色。 Capsanthin mainly used as a food additive, it can make a variety of food coloring in a variety of hues; widely used in medicine, cosmetics and other poultry and poultry feed production in advanced; abroad have been widely used in textile dyeing, as well as coloring paints, plastics . 辣椒精主要用于食品工业的原料,可作餐馆、食堂、家庭常备佐料,或直接用于烹饪调味调色等;最重要的用途是作辣椒防卫喷剂和对付狗、熊、蛇等危险动物的驱逐剂; 国内外已大量用于生产辣椒痛可贴、辣椒止痛膏等外用药膏。 Capsicum main raw material for the food industry, can be used for restaurants, canteens, families standing sauce, or directly used for cooking and other seasoning palette; the most important use is as a defense pepper sprays and deal with dangerous dogs, bears, snakes, etc. animal repellent; at home and abroad have been widely used in the production of pepper pain can paste, chili paste, topical ointments and pain. 目前,从红辣椒中提取分离辣椒碱、辣椒红色素和辣椒精的工艺方法有多种,如溶剂萃取法、超临界萃取法、微波萃取法等。 At present, capsaicin extract isolated from red peppers, paprika oleoresin of Capsicum and process a variety of methods, such as solvent extraction, supercritical fluid extraction, microwave extraction and the like. 超临界萃取法具有分离除杂效果较好,萃取率高、可实现辣椒碱与辣椒红综合开发的优点,但其一次性设«资大,设备属于三类耐压容器,受处理量的限制,产量低,运纟亍费用高, 而且仍然不能完全摆脱有机溶齐啲使用,工业开发难度较大, 一般企4i^隹以采用。 Supercritical extraction has better impurity separation, extraction rate, and advantages of the capsaicin capsanthin comprehensive development can be achieved, but the «disposable its owned set, three types of equipment belonging to the pressure vessel, by the processing amount , low yields, high transport costs Si right foot, but still can not completely get rid of organic solvents Qi GOD use, industrial development more difficult, the general 4i ^ enterprises to adopt short-tailed bird. . 微波萃取法具有萃取速度快、萃取效率高的优点,但该方法加工能力小, 实现工业化困难。 Microwave extraction having extraction speed, the advantages of high extraction efficiency, but the method of small processing capacity, difficulties in industrialization. 溶剂萃取法具有浸取加工能力大、设备简单、易于实现工业化生产,在实际生产中用得最多,但目前的输降取法,首先以混合溶剂或单一溶剂为提取溶剂,把辣椒碱、辣椒红色素和辣椒精从辣椒原料中全部提取出来,得到含辣椒碱、辣椒红色素和辣椒精的混合提取液,经Mffi蒸馏浓縮得到含辣椒碱、辣椒红色素和辣椒精的混合提取物粗产品,然后使用超临界流体萃取技术纯化粗品,或用激瞎取法通过多次萃取和分相分离,分出的辣椒红色素萃取液进行蒸发«后再加入浓烧碱溶舰行分离色素和辣椒碱处理,经过碱化、中和、酸化、分液、洗涤、用除辣剂除辣、脱臭等工序,才能得到辣椒碱、辣椒精和辣椒红色素中1〜2种主要产品。 Leaching solvent extraction with a large processing capacity, the device is simple, easy to realize industrial production, most frequently used in the actual production, but the output of emulated drop, first to a single solvent or a mixed solvent as the extraction solvent, the capsaicin, capsanthin pigments and from capsicum pepper extract out of all of the raw material, obtained containing capsaicin, capsanthin and mixed capsicum extract was concentrated by distillation to give Mffi containing capsaicin, capsanthin and the mixed extract of capsicum crude product and then using a supercritical fluid extraction technique for the purification of crude product, or a plurality of times with a laser blind emulated by extraction and phase separation, the separated extracts were evaporated capsanthin «concentrated caustic solution was added and then ship line separation and the capsaicin treated pigment , basification, neutralization, acidification, liquid separation, washed with hot spicy agent other, in addition to deodorization step, in order to obtain capsaicin, Paprika Oleoresin capsicum, and in 1 to 2 major products. 因此,现有的辣椒深加工工艺,不仅工序繁杂、操作麻烦、效率低,而且经酸碱化学处理过程后,有效成分分子结构遭破坏,提取率低,所提的辣椒色素辣味、异i^n⑩!j残留难脱除,分离精制难度大,生产周期长、损耗大。 Thus, the conventional pepper deep processing, not only complicate the process, the operation is troublesome, inefficient, and after the acid-base chemical treatment, destruction of the molecular structure of active ingredient, low extraction rate, referred spicy pepper pigment, iso-i ^ n⑩! j residue Away addition, isolation and purification difficult, long production cycle, a large loss. 发明内容本发明的目的是提出一种从红辣椒中提取分离辣椒碱、辣椒红色素和辣椒精粗产品的工艺方法,以解决现有翻降取法存在的缺点。 Object of the present invention is to provide an extract from red pepper capsaicin, capsicum capsanthin forage to concentrate and process for separating products, in order to solve the drawbacks of the conventional flip down emulated presence. 本发明根据辣l叔的化学成分及其含量、有效成分和杂质成分的分子结构及理化性质等,采取一种新的提取分离技术和工艺路线,即以粉碎成一定粒度的干红辣椒为原料,以含水乙醇为提取剂,采取三段提取法,控制工艺条件,先后得至幌椒碱、辣椒精和辣椒红色素三种提取物,使它们在提取阶段即得到分离,省去了后序工段中辣椒碱与辣椒红色素难分离的麻烦;在提取阶段用同一提取罐和同种溶剂提取分离三种提取物,而且不用碱溶、酸化处理,临界流体萃取设备或柱层析分离工艺,有利于提高辣椒红色素和辣椒碱的产出率和降低生产成本;成功地解决了用溶剂法提取辣椒红色素和辣椒碱时经常遇到的提取率低,色素难除辣、分离除杂麻烦,产品中溶剂残留高和异味重等几大难题。 According to the present invention the chemical composition and the content of hot-t l, the molecular structure and physicochemical nature of the active ingredient and the impurities, to adopt a new extraction and separation process route, i.e. crushed into a certain size as a raw material of red pepper , as an aqueous alcohol extractant to take three-stage extraction, controlling the process conditions has to have a base Sapporo pepper, capsicum extract, and three kinds of red pigment, i.e., that they be separated at the extraction stage, eliminating the need for subsequent paprika oleoresin capsaicin station and difficult to separate the trouble; the same extraction phase was extracted with the same solvent extraction tank and three extracts were separated, but not alkali-soluble, acid treatment, supercritical fluid extraction process equipment or column chromatography, help to improve the yield of red pigment and pepper alkali and reduce production costs; successfully resolved the low extraction rate often encountered when extracting red pigment and pepper alkali solvent method, in addition to spicy pigment difficult to separate impurity trouble , height and weight residual solvent odor in the product and other major problems. 本发明具有工艺简单、易操作控制,设备投资少、溶剂易回收再利用、成本低、 周期短,有效成分收率高、顿合工业化规模生产靴点。 The present invention has simple process, easy to operate and less control, investment in equipment, easily recyclable solvent, low cost, short cycle, the active ingredient high yield, industrial scale production Dayton shoe engagement point. 本发明的目的任务是这样实施的:以粉碎成一定茅娘的干红辣椒为原料,以含水乙醇为提取剂,采取三段提取法,通过调控提取翻的浓度和加入量、提取温度、提取时间工艺条件,先后得到辣椒碱、辣椒精和辣椒红三种提取液, 再将三种提取液分别进行MJH缩和蒸馏,回收溶齐御除去溶剂残留,制得辣椒碱、辣椒红色素和辣椒精三种粗产品。 Object of the object of the present invention is implemented: to crush into a certain Mao mother red pepper as raw materials, an aqueous ethanol as extractant, to take three-stage extraction, extraction by regulating the concentration and amount of translation, extraction temperature, time conditions, has been capsaicin, and red pepper and capsicum extract, then the extract were three kinds MJH condensing and distillation, recycling the solvent was removed the residue was dissolved Yu Qi, prepared capsaicin, capsanthin and pepper three kinds of refined crude products. 可根据它们的不同用途再制得不同规格等级的辣椒碱、辣椒红色素和辣椒精工业产品。 Capsaicin may be further prepared according to their use of different levels of different specifications, Capsicum capsanthin and industrial products. 具体实施方式本发明采取的技术措施和具体实施方式如下-本发明戶;MH段提取法制备辣椒碱、辣椒精和辣椒妊种提取液的内容为: 其第一段是在放有一定量红辣椒原料的提取容器中,按l : 8〜12的重量比加入浓度为50%〜80%的乙醇溶液,在30。 DETAILED technical measures taken by the embodiment of the present invention and embodiments as follows - the user of the present invention; MH segment content prepared capsaicin extract, and Capsicum pepper extract is a kind of pregnancy: the first section which is placed in the amount of red pepper raw material extraction vessel, by l: 8~12 weight ratio of the added concentration of 50% ~ 80% ethanol, at 30. C〜60。 C~60. C的驢下浸提4〜6小时,乡纽滤得辣椒碱提取液;其第二段是按1 : 6〜10的重量比往提取容器中加入浓度为80%〜95%的乙醇溶液,在70。 Ass leaching of C 4 ~ 6 hours, Township New capsaicin extract was filtered; the second is 1: 6~10 weight ratio of concentrations are added to the extraction vessel is 80% ~ 95% ethanol solution, 70. C〜90。 C~90. C的鹏下热回流提取1〜3小时,经过滤得辣椒精提取液;其第三段是按1 : 4〜8的重量比往提取容器中加入浓度为85%〜95%的乙醇溶液,在65。 Peng thermal reflux extraction C ~ 3 hours, filtered to give Capsicum extract; the third section is 1: 4 to 8 weight ratio of concentrations are added to the extraction vessel is 85% ~ 95% ethanol solution, 65. C〜85。 C~85. C的鹏下热回流提取0.5〜2.5小时,经过滤得辣椒红提取液。 Peng C under reflux heat extraction 0.5~2.5 hours, filtered to give a red pepper extract. 再将三种提取液分别进行Mffi浓縮和蒸馏,回收乙醇溶齐,除去提取物的溶剂残留,制得辣椒碱、辣椒红色素和辣椒精三种粗产品。 Then three kinds Mffi extracts were concentrated and distilled, recovering ethanol homogeneous solution, the solvent was removed the residue was extracted was prepared capsaicin, capsanthin, and three kinds of Capsicum crude product. 实施例l:在放有一定量红辣椒原料的提取容器中,按l : 12的重量比加入浓度为50% 的乙醇溶液,在6(TC的離下浸提4小时,乡劍滤得辣椒^l取液;再按l :6 的重量比往提取容器中加入浓度为95%的乙醇溶液,在90。C的温度下热回流提取1小时,经过滤得辣椒精提取液;最后按1 : 8的重量比往提取容器中加入浓度为85%的乙醇溶液,在65。C的離下热回流提取2.5小时,经过滤得辣椒红提取液。再将三种提取液分别进行鹏«和蒸馏,即将三种提取液分别置于Mffi浓縮罐和薄膜蒸发器中进行歉缩和蒸馏脱残,回收乙醇辭诉卩除去提取物的敏u残留,可制得辣椒碱、辣椒红色素和辣椒精三种粗产品。实施例2:在放有一定量红辣椒原料的提取容器中,按1 : 8的重量比加入浓度为80% 的乙醇溶液,在3(TC的離下浸提6小时,^!滤得辣椒鹏取液;再按l: 10的重量比往提取容器中加入浓度为80% Example l embodiments: the discharge a quantity extraction vessel paprika raw material, by l: weight 12 ratio added at a concentration of 50% ethanol, (the TC of from leached for 4 hours and rural sword The filtered peppers 6 ^ l extract solution; then l: 6 by weight ethanol extract was added to the vessel over 95% concentration to heat extraction at a temperature of 90.C reflux for 1 hour, filtered to give capsicum extract; and finally 1: the weight ratio of 8 was added to the extraction vessel at a concentration of 85% ethanol solution, extracting heat from at 65.C to reflux for 2.5 hours, filtered to give a red pepper extract. extracts were then three kinds Peng «and distillation , i.e. three kinds of extract were placed Mffi concentration tank and a thin film evaporator for condensing and distilling off residual apology, recovering ethanol extract speech removed sensitive u v Jie residue, can be prepared capsaicin, capsanthin and pepper fine three kinds of crude product Example 2: in a container placed an amount of the extraction of raw red pepper, 1: 8 weight ratio added at a concentration of 80% ethanol solution, 3 (TC ex extraction for 6 hours, ! ^ Peng pepper extract solution obtained was filtered; then l: 10 by weight ratio is added to a concentration of 80% extraction vessel 的乙醇溶液,在7(TC的温度下热回流提取3小时,经过滤得辣椒精提取液;最后按1 : 4的重量比往提取容器中加入浓度为95%的乙醇溶液,在85"€的鹏下热回流提取0.5小时,经过滤得辣椒红提取液。再将三种提取液分别进行鹏鄉和蒸馏,即将三种提取液分另擅于鹏浓縮罐和薄膜蒸发器中进行浓縮和蒸馏脱残,回收乙醇溶剂和除去提取物的溶剂残留,可制得辣椒碱、辣椒红色素和辣椒精三种粗产品。实施例3:在放有一定量红辣椒原料的提取容器中,按l : 10的重量比加入浓度为65% 的乙醇溶液,在40。C的離下浸提5小时,乡纽滤得辣椒鹏取液;再按l :7的重量比往提取容器中加入浓度为85%的乙,液,在80。C的、皿下热回流提取2小时,经过滤得辣ii精提取液;最后按1 : 5的重量比往提取容器中加入浓度为90%的乙醇溶液,在75°(3的離下热回流提取1.5小时,经过滤得辣椒 Ethanol solution, extracted 7 (heat to reflux temperature TC for 3 hours, filtered to give Capsicum extract; and finally 1: 4 weight ratio to the extraction vessel was added an ethanol solution of a concentration of 95%, in the 85 "€ Peng 0.5 hours under heat reflux extraction, the extract was filtered to give red pepper. then three kinds of extracts were distilled and Peng Township, i.e. three extracts were concentrated Peng good at the other points can be thin film evaporator and concentrated condensing and distilling off residual ethanol recovery solvent and the residual solvent removed extract, capsaicin can be prepared, three kinds of red pigment and capsicum crude product Example 3: extraction vessel placed in a certain amount of raw red pepper, by l: 10 weight ratio was added at a concentration of 65% ethanol solution for 5 hours at 40.C leached away, Township New Peng pepper extract solution obtained was filtered; then l: 7 by weight ratio of extract added to the vessel acetate concentration of 85%, liquid, extraction, hot dish 80.C for 2 hours at reflux, filtered hot to obtain refined extract ii; final 1: 5 weight ratio of the extraction vessel to a concentration of 90% was added ethanol solution, at 75 ° (1.5 hours to extract heat from the reflux 3, pepper filtered to give 曰再将三种提取液分别进行Mffi鄉和蒸馏,即将三种提取液分另擅于鹏浓縮罐和薄膜蒸发器中进行浓縮和蒸馏脱残,回收乙醇溶剂和除去提取物的溶剂残留,可制得辣椒碱、辣椒红色素和辣椒精三种粗产品。 Said three kinds of extracts were then Mffi rural and distillation, i.e. good at other points three extracts were concentrated Peng thin film evaporator and can be concentrated and distilled off the residue, the solvent was removed and the solvent recovering ethanol extract residues , capsaicin can be prepared, three kinds of red pigment and capsicum crude product.

Claims (2)

  1. 1、一种从红辣椒中提取分离辣椒碱、辣椒红色素和辣椒精粗产品的工艺方法,其特征在于:以粉碎成一定粒度的红辣椒为原料,以含水乙醇为提取溶剂,采取三段提取法制备辣椒碱、辣椒精和辣椒红色素三种提取液,即在同一个提取容器中加入一定量红辣椒原料,通过调控提取剂浓度和加入量、提取温度、提取时间,先后得到辣椒碱、辣椒精和辣椒红色素三种提取液,使它们在提取阶段即行分离;再将三种提取液分别进行减压浓缩和蒸馏,回收溶剂和除去溶剂残留,制得辣椒碱、辣椒红色素和辣椒精三种粗产品。 A capsaicin extract, capsanthin and process for separating the product from forage to concentrate pepper red pepper, characterized in that: to crush into a certain size of red pepper as raw materials, an aqueous ethanol as solvent, taking three sections Preparation of capsaicin extract, capsanthin, and three kinds of capsicum extract SYSTEM, i.e. in the same extraction vessel by adding an amount paprika starting material, by regulating the amount and concentration of the extraction agent, the extraction temperature, extraction time, capsaicin has been , capsicum extract, and three kinds of red pigment, i.e., the extraction phase so that they line separation; and then three kinds of extracts were concentrated and distilled under reduced pressure to recover the solvent and residual solvent was removed, to obtain capsaicin, capsanthin and capsicum three kinds of crude product.
  2. 2、 根据权利要求1戶,的从红辣椒中提取分离辣椒碱、辣椒红色素和辣椒精粗产品的工艺方法,其特征在于:所述的三段提取法制备辣椒碱、辣椒精和辣椒红色素三种提取液的工艺为:其第一段是在放有一定量红辣椒原料的提取容器中,按1 : 8〜12的重量比加入浓度为50%〜80%的乙醇溶液,在30°C〜60 。 2, capsaicin extract, capsanthin and process for separating the product from forage to concentrate pepper red pepper according to claim 1, characterized in that: Preparation of three sections capsaicin extract, red pepper and Capsicum said process for the pigment extract three kinds: the first section which is placed in the extraction vessel a certain amount of raw red pepper, 1: 8~12 weight ratio added at a concentration of 50% ~ 80% ethanol solution at 30 ° C~60. C的鹏下浸提4〜6小时,经过滤得辣椒鹏取液;其第二段是按1 : 6〜10 的重量比往提取容器中加入浓度为80%〜95%的乙醇溶液,在7(TC〜90。C的m 下热回流提取1〜3小时,乡纽滤得辣椒精提取液;其第三段是按1 : 4〜8的重量比往提取容器中加入浓度为85%〜95%的乙醇溶液,在65。C〜85。C的温度下热回流提取0. 5〜2. 5小时,经过滤得辣椒红色素提取液。 C is 4 ~ 6 hours Peng leached, dried and filtered to give Peng pepper extract solution; the second is 1: 6~10 weight ratio of concentrations are added to the extraction vessel is 80% ~ 95% ethanol solution, thermal reflux extraction at 7 (TC~90.C of m 1~3 hours, Township New capsicum extract obtained was filtered; the third section is 1: 4 to 8 weight ratio of concentrations are added to the extraction vessel 85% ~ 95% in ethanol, 0.5 5~2 thermal reflux extraction. 65.C~85.C temperature for 5 hours, the extract was filtered to obtain red pigment.
CN 200710300024 2007-12-21 2007-12-21 Process for extracting and separating capsaicin, capsicum red pigment and capsicum oleoresin crude product from red pepper CN101225052B (en)

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CN102060728A (en) * 2010-12-20 2011-05-18 重庆市农业科学院 Method for extracting capsorubin and capsaicin from chillies
CN101665446B (en) 2009-09-25 2012-06-27 四川汇科生物技术有限公司 Extract method of capsaicine and capsanthin
CN101619028B (en) 2009-06-17 2012-06-27 刘春巧 Method for preparing capsicine monomer
CN103146224A (en) * 2013-03-20 2013-06-12 湖南农业大学 Method for directly producing non-spicy haematochrome from fresh chili pepper
CN103910646A (en) * 2014-04-14 2014-07-09 蒋悦茜 Method for extracting capsaicin and capsanthin from capsicum oleoresin
CN104830096A (en) * 2015-04-21 2015-08-12 河北东之星生物科技股份有限公司 Method for preparation of high light absorption ratio capsorubin
CN104920912A (en) * 2015-07-11 2015-09-23 青岛赛特香料有限公司 Method for preparing feed additives containing capsanthin sedimentation slags

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CN101619028B (en) 2009-06-17 2012-06-27 刘春巧 Method for preparing capsicine monomer
CN101665446B (en) 2009-09-25 2012-06-27 四川汇科生物技术有限公司 Extract method of capsaicine and capsanthin
CN102060728A (en) * 2010-12-20 2011-05-18 重庆市农业科学院 Method for extracting capsorubin and capsaicin from chillies
CN103146224A (en) * 2013-03-20 2013-06-12 湖南农业大学 Method for directly producing non-spicy haematochrome from fresh chili pepper
CN103146224B (en) 2013-03-20 2014-05-07 湖南农业大学 Method for directly producing non-spicy haematochrome from fresh chili pepper
CN103910646A (en) * 2014-04-14 2014-07-09 蒋悦茜 Method for extracting capsaicin and capsanthin from capsicum oleoresin
CN104830096A (en) * 2015-04-21 2015-08-12 河北东之星生物科技股份有限公司 Method for preparation of high light absorption ratio capsorubin
CN104830096B (en) * 2015-04-21 2016-10-12 河北东之星生物科技股份有限公司 A method for a high extinction ratio capsanthin Preparation
CN104920912A (en) * 2015-07-11 2015-09-23 青岛赛特香料有限公司 Method for preparing feed additives containing capsanthin sedimentation slags

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