WO2015109657A1 - 一种原位富集制备天然玉米黄素的方法 - Google Patents

一种原位富集制备天然玉米黄素的方法 Download PDF

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WO2015109657A1
WO2015109657A1 PCT/CN2014/074707 CN2014074707W WO2015109657A1 WO 2015109657 A1 WO2015109657 A1 WO 2015109657A1 CN 2014074707 W CN2014074707 W CN 2014074707W WO 2015109657 A1 WO2015109657 A1 WO 2015109657A1
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solid adsorbent
zeaxanthin
solvent
extraction
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邹汉法
靳艳
张宇
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Dalian Institute of Chemical Physics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
    • C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00—Systems containing only non-condensed rings
    • C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated

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  • the invention relates to a method for extracting natural zeaxanthin, in particular to a method for extracting and preparing zeaxanthin from vegetables and fruits by in situ enrichment method, and the preparation method of zeaxanthin of the invention has simple process, high efficiency and solvent Low use and high purity of zeaxanthin.
  • the prepared natural zeaxanthin can be used in the fields of foods, health foods, medicines, cosmetics, and the like. Yes
  • Zeaxanthin has two chiral carbons at 3 and 3', corresponding to four isomers, respectively (3R, 3'S)-, (3S, 3'R)-, (3R, 3'R) -, (3S, 3'S) - zeaxanthin. Since the molecular structure of zeaxanthin is symmetrical, (3R, 3'S)-, (3S, 3' R)-zeaxanthin has the same structure and is called meso-zeaxanthin.
  • the zeaxanthin in nature is in the form of 3R, 3'R- zeaxanthin, and the corn yellow which is chemically synthesized from lutein is meso-zeaxanthin.
  • Zeaxanthin and lutein are the only carotenoids in the macular area of the human retina and are the major constituent pigments of the macular pigment (Clinics in Dermatology (2009) 27, 195-201). Zeaxanthin is mainly concentrated in the center of the macular area of the retina, and lutein is found throughout the retina. Zeaxanthin has a specific function of absorbing blue light in ultraviolet rays, and can avoid blue light damage to the retina. Meanwhile, zeaxanthin and lutein also have anti-oxidation effects, and can prevent eye damage caused by oxidation of retina, epithelial cells, choroid, and the like.
  • zeaxanthin and lutein have important effects on human vision and nutritional protection of the eye (Br J Ophthalmol 1999 83: 867-877). Experiments have shown that zeaxanthin is more important than the effect of lutein on the eye. When the supply of zeaxanthin is insufficient, the body will automatically convert lutein into zeaxanthin.
  • Age-related macular degeneration is the primary eye disease for visual impairment and blindness in the elderly.
  • AMD Age-related macular degeneration
  • the risk of AMD is closely related to the concentration of zeaxanthin and lutein in human blood.
  • a large number of studies have shown that 6 mg of zeaxanthin and leaves are taken daily.
  • Flavin can effectively reduce the risk of age-related macular degeneration and slow the progression of age-related macular degeneration.
  • Macular pigmented corn Flavin and lutein can also improve eye aversion, glare recovery, dusk dawn vision, dark reaction and other eye problems (Aca demy of Ophthalmic Education).
  • the human body cannot synthesize zeaxanthin by itself. It can only be taken through food. Zeaxanthin is mainly found in corn, pepper, egg yolk and dark green vegetables, but the content of zeaxanthin in dark green vegetables is much lower than lutein. For AMD high-risk populations, relying solely on obtaining zeaxanthin from food is very limited and requires additional supplements to supplement zeaxanthin.
  • the US FDA evaluated the safety of zeaxanthin, with a daily maximum of 160 mg for humans and a recommended amount of zeaxanthin 6 mg/day for the prevention of AMD and visual fatigue.
  • the zeaxanthin in nature is in the form of 3R, 3'R-zeaxanthin, and the experimental data for the safety of zeaxanthin is also based on 3R, 3'R-zeaxanthin.
  • the resources of zeaxanthin are very limited.
  • zeaxanthin on the market is mainly obtained from lutein by chemical synthesis.
  • the zeaxanthin obtained by chemical method is meso-zeaxanthin, which has not yet been seen.
  • - Safety report of zeaxanthin From a safety point of view, 3R, 3'R-zeaxanthin extracted directly from plants is the safest and most reliable. (Food and Chemical Toxi cology 49 (2011) 2841-2848 )
  • the object of the present invention is to provide a method for extracting and preparing natural zeaxanthin; the method of the invention enriches natural zeaxanthin obtained by extraction and saponification in situ by a solid adsorbent, which reduces the separation and purification of zeaxanthin
  • the required steps greatly reduce the use of solvents and water, and the obtained natural zeaxanthin has high purity and can be applied to food, health food, medicine and the like, and has good industrial application prospects.
  • the technical scheme adopted by the present invention is as follows - a technique for preparing natural zeaxanthin by in-situ enrichment method, and after saponification of the raw material rich in zeaxanthin, a solid adsorbent is directly added to the saponification liquid to carry out the original method.
  • the enrichment is carried out, and the zeaxanthin is eluted with a small amount of solvent, and the eluate is concentrated and dried to obtain a higher content of zeaxanthin.
  • step 2) according to the operation process of step 1), the filter residue obtained in the previous step is extracted again, and the extraction is repeated 2-4 times;
  • the medium adsorbent is slowly shaken by adding a medium-polar solvent, and the solid adsorbent is removed by standing, and the obtained solvent is concentrated and dried to obtain a natural zeaxanthin product.
  • Step 2) according to the operation process of step 1), the filter residue obtained in the previous step is extracted again, and the extraction is repeated 2-4 times;
  • the precipitate was separated by static filtration; the extract and the residue were obtained.
  • the plant refers to one or more of the fruits, scorpions, roots, stems, leaves, flowers or whole plants of the plant; the plants used are alfalfa, brocade, corn, pepper, sea buckthorn, pumpkin, persimmon One or more of them.
  • the extraction solvent is: one or more of methanol, ethanol, propanol, butanol, ethyl acetate, dichloromethane, chloroform, diethyl ether, acetone, cyclohexane, n-hexane, petroleum ether. Solvent mixture;
  • the medium polar solvent is: methanol, ethanol, propanol, butanol, ethyl acetate, dichloromethane, trichloromethane, One or more of diethyl ether and acetone;
  • the solid adsorbent is one or more of silica, hydroxypropyl dextran gel, and polystyrene resin.
  • the alcohol in the alcohol solution in the steps 3) and 4) is one or more of methanol, ethanol, and propylene glycol.
  • the amount of the solid adsorbent added after the saponification is completed, the mass of the raw material: the mass of the solid adsorbent 1: 0.1-10.
  • the preparation method is as follows:
  • step 2) according to the operation process of step 1), the filter residue obtained in the previous step is extracted again, and the extraction is repeated 2-4 times;
  • solid adsorbent mass 1: 0.5-8; slowly stirred for 0.5 to 10 hours, and allowed to stand for separation to obtain natural zeaxanthin.
  • a solid adsorbent the solid adsorbent rich in natural zeaxanthin is washed with a deionized water or an alcohol solution at 20 to 50 ° C until the pH is neutral, and the solution is removed;
  • step 2) according to the operation process of step 1), the filter residue obtained in the previous step is extracted again, and the extraction is repeated 3 times;
  • solid adsorbent mass 1: 1; slowly stirred for 2 hours, and allowed to stand for separation to obtain a solid adsorbent enriched with natural zeaxanthin. Flushing the solid adsorbent rich in natural zeaxanthin to a neutral pH with deionized water or an alcohol solution at 40 ° C to remove the solution;
  • the in-situ enrichment method reduces the traditional method of using water to elute alkali, which reduces the discharge of wastewater; the enriched zeaxanthin can be eluted with a small amount of solvent, reducing the amount of organic solvent used, and is environmentally friendly.
  • the product has a high content of zeaxanthin.
  • the zeaxanthin content prepared by the preparation process of the present invention can be up to 90% or more.
  • Zeaxanthin is the main component of human macular pigment. Supplementing zeaxanthin can prevent eye diseases such as age-related macular degeneration, cataract, and has a good alleviation effect on eye fatigue. Zeaxanthin also has a sunscreen effect, and natural extracted zeaxanthin has high safety, so it has good application prospects in the fields of food, health care products, medicines, cosmetics and the like.
  • Figure 1 is a mass spectrum of zeaxanthin of Example 1 of the present invention.
  • Example 2 is a nuclear magnetic resonance spectrum of zeaxanthin according to Example 1 of the present invention.
  • Fig. 3 is a liquid chromatogram of zeaxanthin of Example 1 of the present invention (* is zeaxanthin in the figure).
  • zeaxanthin was prepared according to the following process:
  • the filter residue was further added with 10 liters of ethyl acetate for the second extraction; the extraction was carried out at 30 ° C for 2 hours; after the end of the extraction, the precipitate was allowed to stand for separation; the extract and the filter residue were obtained;
  • zeaxanthin was prepared according to the following process:
  • the filter residue is again added with 50 liters of acetone for the second extraction; the mixture is stirred and extracted at 60 ° C for 5 hours; after the end of the extraction, the precipitate is separated; the extract and the filter residue are obtained;
  • Example 3 To the solid adsorbent, 100 liters of a mixed solvent of diethyl ether and ethyl acetate was added, and the mixture was shaken slowly, and the mixture was allowed to stand for separation to remove the solid adsorbent. The obtained solvent was concentrated and dried to obtain 30 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, Nuclear magnetic resonance spectroscopy, liquid chromatography, etc. proved that the obtained product was zeaxanthin, and the purity was 68%.
  • zeaxanthin was prepared according to the following process:
  • the pepper is freeze-dried, ground into a powder, passed through a 100 mesh sieve, and 1000 g of the sieved powder is taken.
  • solvent volume lg: 100 ml
  • a mixed solvent of petroleum ether and methylene chloride is added (volume ratio 1:1).
  • the filter residue is again added to 100 liters of petroleum ether and dichloromethane mixed solvent for the second extraction; the mixture is stirred and extracted at 80 ° C for 1 hour; after the end of the extraction, the precipitate is allowed to stand for separation; the extract and the filter residue are obtained;
  • a solid adsorbent 5 kg of silica, was added, and the mixture was slowly stirred for 1 hour, and allowed to stand for separation to obtain a solid adsorbent rich in natural zeaxanthin; the natural zeaxanthin-rich material was enriched with an ethanol solution at 20 ° C. The solid adsorbent is washed until the pH is neutral, and the solution is removed;
  • Example 4 To the solid adsorbent, 25 liters of diethyl ether was added and slowly shaken, and the mixture was allowed to stand for separation. The solid adsorbent was removed, and the obtained solvent was concentrated and dried to obtain 25 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance spectrum, liquid The obtained product was confirmed to be zeaxanthin by a phase chromatography or the like, and the purity was 60%.
  • Example 4 To the solid adsorbent, 25 liters of diethyl ether was added and slowly shaken, and the mixture was allowed to stand for separation. The solid adsorbent was removed, and the obtained solvent was concentrated and dried to obtain 25 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance spectrum, liquid The obtained product was confirmed to be zeaxanthin by a phase chromatography or the like, and the purity was 60%.
  • Example 4 To the solid
  • zeaxanthin was prepared according to the following process:
  • the brocade lanterns were freeze-dried and ground into powder. After passing through a 100 mesh sieve, 1000 g of the sieved powder was taken, 50 liters of a mixed solvent of methanol and ethyl acetate was added, and the mixture was stirred at 50 ° C for 8 hours, and the precipitate was allowed to stand after the extraction. Separating; obtaining extract and filter residue;
  • the filter residue is further added with 50 liters of a mixed solvent of methanol and ethyl acetate for the second extraction; and the mixture is stirred and extracted at 50 ° C for 5 hours; after the end of the extraction, the precipitate is allowed to stand for separation; the extract and the filter residue are obtained;
  • Example 5 40 liters of trichloroethane was added to the solid adsorbent and shaken slowly, and the solid adsorbent was removed by static separation. The obtained solvent was concentrated and dried to obtain 60 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance The product obtained by spectrum, liquid chromatography, etc. proved to be zeaxanthin with a purity of 75%.
  • Example 5 40 liters of trichloroethane was added to the solid adsorbent and shaken slowly, and the solid adsorbent was removed by static separation. The obtained solvent was concentrated and dried to obtain 60 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance The product obtained by spectrum, liquid chromatography, etc. proved to be zeaxanthin with a purity of 75%.
  • Example 5 40 liters of trichloroethane was added to the solid adsorb
  • zeaxanthin is prepared according to the following process:
  • the corn is freeze-dried, ground into a powder, passed through a 100 mesh sieve, and 1000 g of the sieved powder is taken, 20 liters of a mixed solvent of petroleum ether and ethyl acetate is added, and the mixture is stirred and extracted at 30 ° C for 5 hours, and after standing, the precipitate is separated and allowed to stand; Obtaining extract and filter residue;
  • the filter residue is further added to a mixed solvent of petroleum ether and ethyl acetate, 20 liters for the second extraction; 30 ° C, stirring and extraction for 5 hours; after the end of the extraction, the precipitate is allowed to stand for separation; the extract and the filter residue are obtained;
  • Example 6 1 liter of trichloroacetic acid was added to the solid adsorbent and shaken slowly, and the solid adsorbent was removed. The solvent was concentrated and dried to obtain 36 g of natural zeaxanthin product. The same method as in Example 1 was carried out: mass spectrometry, nuclear magnetic resonance The product obtained by spectrum, liquid chromatography, etc. proved to be zeaxanthin, and the purity was 60%.
  • the zeaxanthin was prepared by the following process using loquat fruit and loquat leaves as raw materials: The loquat fruit and the loquat leaves were freeze-dried, ground into a powder, passed through a 100 mesh sieve, and 1000 g of the sieved powder was taken. 80 liters of a mixed solvent of n-hexane and ethanol (1:1 by volume) was added, and the mixture was stirred at 35 ° C for 4 hours. , after the end of the extraction, the precipitate is separated by standing; the extract and the filter residue are obtained;
  • the filter residue was again added with a mixed solvent of n-hexane and ethanol (1:1 by volume) for the second extraction; and the mixture was stirred at 5 ° C for 4 hours; after the end of the extraction, the precipitate was allowed to stand for separation; the extract and the residue were obtained;
  • zeaxanthin is prepared according to the following process:
  • the filter residue is again added to a mixed solvent of petroleum ether and n-hexane, 60 liters for the second extraction; and the extraction is carried out for 5 hours; after the end of the extraction, the precipitate is allowed to stand for separation; the extract and the filter residue are obtained;
  • Example 8 To the solid adsorbent, 300 ml of ethyl acetate was added and shaken slowly, and the mixture was allowed to stand for separation to remove the solid adsorbent. The obtained solvent was concentrated and dried to obtain 26 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance spectroscopy The liquid chromatogram and the like proved that the obtained product was zeaxanthin, and the purity was 69%.
  • Example 8 To the solid adsorbent, 300 ml of ethyl acetate was added and shaken slowly, and the mixture was allowed to stand for separation to remove the solid adsorbent. The obtained solvent was concentrated and dried to obtain 26 g of natural zeaxanthin product by the same method as in Example 1: mass spectrometry, nuclear magnetic resonance spectroscopy The liquid chromatogram and the like proved that the obtained product was zeaxanthin, and the purity was 69%.
  • Example 8 To the solid ad
  • zeaxanthin was prepared according to the following process:
  • the persimmon is freeze-dried, ground into a powder, passed through a 100 mesh sieve, and 1000 g of the sieved powder is taken, 50 liters of ethyl acetate is added, and the mixture is stirred and extracted at 35 ° C for 3 hours. After the end of the extraction, the precipitate is allowed to stand for separation; the extract and the residue are obtained. ;
  • the filter residue was further added with 50 liters of ethyl acetate for the second extraction; and the mixture was stirred and extracted at 35 ° C for 3 hours; after the end of the extraction, the precipitate was allowed to stand for separation; the extract and the filter residue were obtained;
  • seabuckthorn was freeze-dried and ground into a powder. After passing through a 100 mesh sieve, 1000 g of the sieved powder was taken, 20 liters of methanol was added, and the mixture was stirred at 40 ° C for 2 hours. Separating and separating the precipitate; obtaining an extract and a filter residue;
  • the filter residue is further added with 20 liters of methanol for the second extraction; the mixture is stirred and extracted at 40 ° C for 2 hours; after the end of the extraction, the precipitate is separated; the extract and the filter residue are obtained;
  • the zeaxanthin was prepared by the following process using brocade fruits and oysters as raw materials:
  • the brocade fruit and the hibiscus are freeze-dried and ground into a powder. After passing through a 100 mesh sieve, 1000 g of the sieved powder is taken, 2 liters of acetone is added, and the mixture is stirred and extracted at 90 ° C for 5 hours. After the end of the extraction, the precipitate is allowed to stand for separation; And the filter residue; the filter residue is further added with 2 liters of acetone for the second extraction; and the extraction is carried out at 90 ° C for 5 hours; after the end of the extraction, the precipitate is allowed to stand for separation; the extract and the filter residue are obtained;

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Abstract

本发明涉及天然玉米黄素的制备方法，具体地说是从植物中提取、皂化制备天然玉米黄素，利用固体吸附剂原位富集玉米黄素，干燥后得到纯度较高的天然玉米黄素。本发明采用固体吸附剂原位富集玉米黄素的方法，可大量减少水和有机溶剂的用量，工艺简单、效率高、易于工业放大，可应用于食品、保健食品、药品、化妆品等领域，具有良好的工业应用前景。

Description

一种原位富集制备天然玉米黄素的方法 技术领域
本发明涉及天然玉米黄素的提取方法，具体地说是原位富集法从蔬菜及水果中提取、 制备玉米黄素的方法， 本发明的玉米黄素制备方法具有工艺简单、 效率高、溶剂使用量 少、 玉米黄素纯度高的特点。 所制备的天然玉米黄素可用于食品、 保健食品、 药品、 化 妆品等领域。 是 带
Figure imgf000002_0001
玉米黄素有两个手性碳位于 3和 3'， 对应有四个同分异构体， 分别是 (3R,3'S)-， （3S, 3'R)-， （3R,3'R) -,(3S,3'S)-玉米黄素。 由于玉米黄素分子结构对称， （3R,3'S)-， （3S,3' R)-玉米黄素的结构完全相同， 被称为 meso-玉米黄素。 自然界中的玉米黄素是以 3R,3'R- 玉米黄素的形式存在， 以叶黄素为原料通过化学法合成的玉米黄色均为 meso-玉米黄素。
玉米黄素与叶黄素是人体视网膜的黄斑部位唯一的类胡萝卜素，是黄斑色素的主要 组成色素（Clinics in Dermatology (2009) 27, 195-201 ) 。 玉米黄素主要集中在视网膜 的黄斑区中心，叶黄素则遍及视网膜。玉米黄素具有特异性的吸收紫外线中蓝光的作用， 可避免蓝光对视网膜损伤，同时玉米黄素和叶黄素还具有抗氧化的作用，可防止视网膜、 上皮细胞、脉络膜等由于氧化引起的眼损伤， 因此玉米黄素和叶黄素对于人体视力和眼 睛的营养保护具有重要的作用（Br J Ophthalmol 1999 83: 867-877 )。实验证明玉米黄 素比叶黄素对于眼睛的作用更为重要， 当玉米黄素供应不足时人体会将叶黄素自动转化 为玉米黄素。
老年性黄斑变性（AMD)是老年人视力障碍和致盲的首要眼病， AMD的患病风险 与人体血液中的玉米黄素和叶黄素浓度密切相关， 大量研宄证明每日摄入 6mg玉米黄素 和叶黄素可有效降低老年性黄斑变性风险， 减缓老年性黄斑变性进程。黄斑性色素玉米 黄素和叶黄素还可改善眼睛畏光、 眩光恢复、 黄昏黎明视觉、 暗反应等眼部问题 （Aca demy of Ophthalmic Education) 。
人体无法自身合成玉米黄素，只能通过食物摄取，玉米黄素主要存在于玉米、辣椒、 蛋黄及深绿色蔬菜中， 但深绿色蔬菜中玉米黄素含量远远低于叶黄素。 对于 AMD高风 险人群仅依靠从食品中获取玉米黄素是非常有限的， 需要额外补充剂补充玉米黄质。美 国 FDA评价了玉米黄素的安全性，人体每日服用上限为 160mg，对于预防 AMD及视疲劳 的推荐量为玉米黄素 6mg/天。 自然界中的玉米黄素是以 3R,3'R-玉米黄素的形式存在， 玉米黄素的安全性实验数据也是基于 3R,3'R-玉米黄素得出的。但是玉米黄素的资源非常 有限， 目前市场上的玉米黄素主要以叶黄素为原料， 通过化学合成的方法获得， 化学法 所得到的玉米黄素是 meso-玉米黄素， 还未见 meso-玉米黄素的安全性报道。 从安全角度 考虑从植物中直接提取的 3R,3'R-玉米黄素是最安全可靠的。 （Food and Chemical Toxi cology 49 (2011) 2841-2848 )
发明内容
本发明的目的是提供一种天然玉米黄素的提取、 制备方法； 本发明的方法将提取、 皂化所得的天然玉米黄素通过固体吸附剂原位富集，该方法减少了玉米黄素分离纯化所 需的步骤， 大大减少溶剂、 水的使用， 所获得的天然玉米黄素纯度高， 可应用于食品、 保健食品、 药品等领域， 具有良好的工业应用前景。
为实现上述目的， 本发明采用的技术方案如下- 原位富集法制备天然玉米黄素的技术， 将富含玉米黄素的原料经提取皂化后， 在皂 化液中直接加入固体吸附剂进行原位富集， 再用少量溶剂将玉米黄素洗脱， 洗脱液浓缩 干燥得到含量较高的玉米黄素。
一种原位富集法制备天然玉米黄素的制备方法-
1 )将植物中的一种或二种以上部位干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg: 10~100ml的比例加入提取溶剂， 30~80°C搅拌提取 1~10小时，提取结束后静置沉淀 过滤分离； 得提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 2-4 次；
3 )合并提取液减压浓缩至溶剂蒸发完， 加入体积为原单次提取溶剂体积的 1/10 1 倍、 质量浓度 1~50%KOH或 NaOH的醇溶液， 10~80°C搅拌皂化 1~40小时；
4)皂化结束后加入固体吸附剂， 缓慢搅拌 0.5~10小时， 静置分离， 得到富集天然 玉米黄素的固体吸附剂； 用 20~50°C的去离子水或醇溶液将富含天然玉米黄素的固体吸 附剂冲洗至所 pH为中性， 除去溶液；
5 ) 固体吸附剂中加入中等极性溶剂缓慢震荡， 静置分离， 除去固体吸附剂， 所得 溶剂浓缩干燥得到天然玉米黄素产品。
所述步骤 2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣再次进行提取， 提取 共重复 2-4次；
再次进行提取过程： 是指将上一步骤所得滤渣再次按照原料质量:溶剂体积 =lg: 10~ 100ml的比例加入上述溶剂进行再次提取， 30~80°C搅拌提取 1~10小时， 提取结束后静 置沉淀过滤分离； 得提取液和滤渣。
所述植物是指植物的果实、宿萼、根、茎、叶、花或整个植株中的一种或二种以上； 所使用的植物为枸杞、 锦灯笼、 玉米、 辣椒、 沙棘、 南瓜、 柿子中的一种或二种以上。
所述提取溶剂为： 甲醇、 乙醇、 丙醇、 丁醇、 乙酸乙酯、 二氯甲烷、 三氯甲烷、 乙 醚、 丙酮、 环己烷、 正己烷、 石油醚中的一种或二种以上的溶剂混合物；
所述中等极性溶剂为： 甲醇、乙醇、丙醇、丁醇、乙酸乙酯、二氯甲烷、三氯甲垸、 乙醚、 丙酮中的一种或二种以上；
所述固体吸附剂为： 二氧化硅、羟丙基葡聚糖凝胶、 聚苯乙烯树脂中的一种或二种 以上。
步骤 3 )和 4) 中的醇溶液中的醇为甲醇、 乙醇、 丙二醇中的一种或二种以上。 皂化结束后加入固体吸附剂的量为， 原料质量： 固体吸附剂质量 =1:0.1~10。
中等极性溶剂的加入量为， 固体吸附剂质量： 中等极性溶剂体积 =lg:2~20ml。
所述的制备方法：
1 )将植物中的一种或二种以上干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg: 10~50ml的比例加入提取溶剂， 30~60°C搅拌提取 1~10小时， 提取结束后静置沉淀过滤 分离； 得提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 2-4 次；
3)合并提取液减压浓缩至溶剂蒸发完， 加入体积为原提取体积的 1/2~1 倍、 质量 浓度 5~30%KOH或 NaOH的醇溶液， 10~60°C搅拌皂化 1~40小时；
4)皂化结束后加入固体吸附剂， 固体吸附剂的加入量为， 原料质量： 固体吸附剂 质量 =1:0.5~8；缓慢搅拌 0.5~10小时，静置分离，得到富集天然玉米黄素的固体吸附剂； 用 20~50°C的去离子水或醇溶液将富含天然玉米黄素的固体吸附剂冲洗至所 pH为中性， 除去溶液；
5)固体吸附剂中加入中等极性溶剂，中等极性溶剂的加入量为：固体吸附剂质量： 中等极性溶剂体积 =lg:2~8ml; 缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓缩 干燥得到天然玉米黄素产品。
所述的制备方法-
1 )将植物中的一种或二种以上干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg: 20ml的比例加入提取溶剂， 40°C搅拌提取 2小时， 提取结束后静置沉淀过滤分离； 得 提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 3 次；
3 )合并提取液减压浓缩至溶剂蒸发完，加入体积为原提取体积的 1倍、质量浓度 1 0%KOH或 NaOH的醇溶液， 40°C搅拌皂化 10小时；
4)皂化结束后加入固体吸附剂， 固体吸附剂的加入量为， 原料质量： 固体吸附剂 质量 =1: 1;缓慢搅拌 2小时，静置分离，得到富集天然玉米黄素的固体吸附剂；用 40°C 的去离子水或醇溶液将富含天然玉米黄素的固体吸附剂冲洗至所 pH为中性，除去溶液；
5)固体吸附剂中加入中等极性溶剂，中等极性溶剂的加入量为：固体吸附剂质量- 中等极性溶剂体积 =lg: 6ml; 缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓缩干 燥得到天然玉米黄素产品。 本发明的特点如下-
1 绿色环保。 原位富集法减少了传统方法使用水洗脱碱的步骤， 减少了废水的排 放； 富集后的玉米黄素用少量溶剂就可洗脱， 减少了有机溶剂的使用量， 具有绿色环保 的特点。
2 产品中玉米黄素含量高。 采用本发明的制备工艺所制备的玉米黄素含量最高可 达到 90%以上。
3 具有良好的应用前景。 玉米黄素是人体黄斑色素的主要成分， 补充玉米黄素可 预防老年性黄斑变性、 白内障等眼部疾病， 而且对于眼疲劳等有很好的缓解作用； 同时 玉米黄素还具有防晒作用，天然提取的玉米黄素安全性高，因此在食品、保健品、药品、 化妆品等领域有良好的应用前景。 附图说明
图 1为本发明实施例 1玉米黄素的质谱图；
图 2为本发明实施例 1玉米黄素的核磁共振氢谱图；
图 3为本发明实施例 1玉米黄素的液相色谱图 （图中 *为玉米黄素)。
具体实施方式
实施例 1
以枸杞果实为原料， 按照以下工艺制备玉米黄素：
取枸杞果实冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 按照枸杞 果实质量:溶剂体积 =lg: 10ml的比例加入乙酸乙酯 10升， 30°C搅拌提取 2小时， 提取结 束后静置沉淀分离； 得提取液和滤渣；
滤渣再次加入乙酸乙酯 10升进行第二次提取； 30°C搅泮提取 2小时； 提取结束后 静置沉淀分离； 得提取液和滤渣；
提取共重复 3次； 合并提取液， 真空浓缩至有机溶剂挥发完， 加入 5升质量浓度 1 0%KOH乙醇溶液， 30°C搅拌皂化 20小时；
皂化结束后加入固体吸附剂一羟丙基葡聚糖凝胶 1000克，缓慢搅拌 0.5小时，静 置分离，得到富集天然玉米黄素的固体吸附剂；用 20°C的去离子水将富含天然玉米黄素 的固体吸附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入 8升乙酸乙酯缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂 浓缩干燥得到天然玉米黄素产品 23克， 通过质谱（图 1)、 核磁共振氢谱（图 2)、 液相 色谱（图 3)， 验证产品中主要成分为玉米黄素， 纯度为 78%。 实施例 2
以锦灯笼果实为原料， 按照以下工艺制备玉米黄素：
取锦灯笼果实冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 按照锦 灯笼果实质量：溶剂体积 =lg:50ml的比例加入丙酮 50升， 60°C搅拌提取 5小时， 提取结 束后静置沉淀分离； 得提取液和滤渣；
滤渣再次加入丙酮 50升进行第二次提取； 60°C搅拌提取 5小时； 提取结束后静置 沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 50升质量浓度 3 0%NaOH甲醇溶液， 60°C搅拌皂化 10小时；
皂化结束后加入固体吸附剂一聚苯乙烯树脂 10公斤， 缓慢搅拌 5小时， 静置分 离，得到富集天然玉米黄素的固体吸附剂；用 20°C的去离子水将富含天然玉米黄素的固 体吸附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入乙醚和乙酸乙酯混合溶剂 100升缓慢震荡， 静置分离， 除去固体 吸附剂，所得溶剂浓缩干燥得到天然玉米黄素产品 30克，通过与实施例 1相同的方法： 质谱、 核磁共振氢谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 68%。 实施例 3
以辣椒为原料， 按照以下工艺制备玉米黄素：
取辣椒冷冻干燥、磨成粉末，过 100目筛子，取筛下粉末 1000克，按照辣椒质量： 溶剂体积 =lg:100ml的比例加入石油醚和二氯甲垸混合溶剂（体积比 1:1 ) 100升， 80°C 搅拌提取 1小时， 提取结束后静置沉淀分离； 得提取液和滤渣； 滤渣再次加入石油醚和二氯甲烷混合溶剂 100升进行第二次提取； 80°C搅拌提取 1 小时； 提取结束后静置沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 10升质量浓度 5 0%KOH乙醇溶液， 80°C搅拌皂化 1小时；
皂化结束后加入固体吸附剂一二氧化硅 5千克， 缓慢搅拌 1小时， 静置分离， 得 到富集天然玉米黄素的固体吸附剂;用 20°C的乙醇溶液将富含天然玉米黄素的固体吸附 剂冲洗至所 pH为中性， 除去溶液；
固体吸附剂中加入乙醚 25升缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓 缩干燥得到天然玉米黄素产品 25克， 通过与实施例 1相同的方法： 质谱、 核磁共振氢 谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 60%。 实施例 4
以锦灯笼宿萼为原料， 按照以下工艺制备玉米黄素：
取锦灯笼宿萼冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入甲 醇和乙酸乙酯的混合溶剂 50升， 50°C搅拌提取 8小时， 提取结束后静置沉淀分离； 得 提取液和滤渣；
滤渣再次加入甲醇和乙酸乙酯的混合溶剂 50升进行第二次提取； 50°C搅拌提取 5 小时； 提取结束后静置沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 40升质量浓度 2 0%NaOH甲醇溶液， 30°C搅拌皂化 20小时；
皂化结束后加入 2000克固体吸附剂一聚苯乙烯树脂， 缓慢搅拌 5小时， 静置分 离，得到富集天然玉米黄素的固体吸附剂；用 30°C的去离子水将富含天然玉米黄素的固 体吸附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入三氯乙烷 40升缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶 剂浓缩干燥得到天然玉米黄素产品 60克， 通过与实施例 1相同的方法： 质谱、 核磁共 振氢谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 75%。 实施例 5
以玉米为原料， 按照以下工艺制备玉米黄素：
取玉米冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入石油醚和 乙酸乙酯的混合溶剂 20升， 30°C搅拌提取 5小时， 提取结束后静置沉淀分离； 得提取 液和滤渣；
滤渣再次加入石油醚和乙酸乙酯的混合溶剂 20升进行第二次提取; 30°C搅拌提取 5 小时； 提取结束后静置沉淀分离； 得提取液和滤渣；
提取共重复 3次;合并提取液，真空浓缩至有机溶剂挥发完，加入 10升质量浓度 5% KOH甲醇溶液， 10°C搅拌皂化 20小时；
皂化结束后加入 500克固体吸附剂一二氧化硅， 缓慢搅拌 2小时， 静置分离， 得 到富集天然玉米黄素的固体吸附剂;用 40°C的乙醇将富含天然玉米黄素的固体吸附剂冲 洗至所 pH为中性， 除去溶剂；
固体吸附剂中加入三氯乙垸 1升缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂 浓缩干燥得到天然玉米黄素产品 36克， 通过与实施例 1相同的方法： 质谱、 核磁共振 氢谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 60%。 实施例 6
以枸杞果实和枸杞叶为原料， 按照以下工艺制备玉米黄素： 取枸杞果实和枸杞叶冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入正己烷和乙醇（体积比 1:1 )的混合溶剂 80升， 35°C搅拌提取 4小时， 提取结束后 静置沉淀分离； 得提取液和滤渣；
滤渣再次加入正己烷和乙醇（体积比 1:1 )的混合溶剂进行第二次提取； 5°C搅拌提 取 4小时； 提取结束后静置沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 40升质量浓度 1 5%KOH乙醇溶液， 25°C搅拌皂化 8小时；
皂化结束后加入 3000克固体吸附剂一羟丙基葡聚糖凝胶， 缓慢搅拌 1小时， 静 置分离，得到富集天然玉米黄素的固体吸附剂；用 40°C的甲醇溶液将富含天然玉米黄素 的固体吸附剂冲洗至所 pH为中性， 除去溶剂；
固体吸附剂中加入二氯甲垸 9升缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂 浓缩干燥得到天然玉米黄素产品 28克， 通过质谱（图 1)、 核磁共振氢谱（图 2)、 液相 色谱（图 3)， 验证产品中主要成分为玉米黄素， 纯度为 82%。 实施例 7
以南瓜和南瓜花为原料， 按照以下工艺制备玉米黄素：
取冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入石油醚与正己 烷（体积比 1:1 ) 的混合溶剂 60升， 40°C搅拌提取 5小时， 提取结束后静置沉淀分离; 得提取液和滤渣；
滤渣再次加入石油醚与正己烷的混合溶剂 60升进行第二次提取;搅拌提取 5小时； 提取结束后静置沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 10升质量浓度 3 5 %NaOH甲醇和乙醇混合溶液， 40°C搅拌皂化 10小时；
皂化结束后加入 100克固体吸附剂一聚苯乙烯树脂， 缓慢搅拌 5小时， 静置分离， 得到富集天然玉米黄素的固体吸附剂;用 40°C的去离子水将富含天然玉米黄素的固体吸 附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入乙酸乙酯 300毫升缓慢震荡， 静置分离， 除去固体吸附剂， 所得 溶剂浓缩干燥得到天然玉米黄素产品 26克， 通过与实施例 1相同的方法： 质谱、 核磁 共振氢谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 69%。 实施例 8
以柿子为原料， 按照以下工艺制备玉米黄素：
取柿子冷冻干燥、磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入乙酸乙酯 5 0升， 35°C搅拌提取 3小时， 提取结束后静置沉淀分离； 得提取液和滤渣；
滤渣再次加入乙酸乙酯 50升进行第二次提取； 35°C搅拌提取 3小时； 提取结束后 静置沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 10升质量浓度 2 0%NaOH甲醇和乙醇混合溶液， 35°C搅拌皂化 10小时；
皂化结束后加入固体吸附剂一聚苯乙烯 1000克， 缓慢搅拌 3小时， 静置分离， 得到富集天然玉米黄素的固体吸附剂;用 35°C的去离子水将富含天然玉米黄素的固体吸 附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入 20升甲醇缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓 缩干燥得到天然玉米黄素产品 21克， 通过质谱（图 1)、 核磁共振氢谱（图 2)、 液相色 谱（图 3)， 验证产品中主要成分为玉米黄素， 纯度为 75%。 实施例 9
以沙棘为原料， 按照以下工艺制备玉米黄素- 取沙棘冷冻干燥、磨成粉末，过 100目筛子，取筛下粉末 1000克，加入甲醇 20升， 40°C搅拌提取 2小时， 提取结束后静置沉淀分离； 得提取液和滤渣；
滤渣再次加入甲醇 20升进行第二次提取； 40°C搅拌提取 2小时； 提取结束后静置 沉淀分离； 得提取液和滤渣；
提取共重复 3次；合并提取液，真空浓缩至有机溶剂挥发完，加入 20升质量浓度 1 0 %NaOH甲醇和乙醇混合溶液， 40°C搅拌皂化 10小时；
皂化结束后加入固体吸附剂一羟丙基葡聚糖凝胶 1000克， 缓慢搅拌 2小时， 静 置分离，得到富集天然玉米黄素的固体吸附剂；用 40°C的去离子水将富含天然玉米黄素 的固体吸附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入 6升甲醇缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓缩 干燥得到天然玉米黄素产品 32克， 通过质谱（图 1 )、 核磁共振氢谱（图 2)、 液相色谱 (图 3 ), 验证产品中主要成分为玉米黄素， 纯度为 95%。 实施例 10
以锦灯笼果实和宿萼为原料， 按照以下工艺制备玉米黄素：
取锦灯笼果实和宿萼冷冻干燥、 磨成粉末， 过 100目筛子， 取筛下粉末 1000克， 加入丙酮 2升， 90°C搅拌提取 5小时， 提取结束后静置沉淀分离； 得提取液和滤渣； 滤渣再次加入丙酮 2升进行第二次提取； 90°C搅拌提取 5小时； 提取结束后静置沉 淀分离； 得提取液和滤渣；
提取共重复 3次； 合并提取液， 真空浓缩至有机溶剂挥发完， 加入 4升质量浓度 6 0%NaOH甲醇溶液， 90°C搅拌皂化 10小时；
皂化结束后加入 80克固体吸附剂一聚苯乙烯树脂，缓慢搅拌 5小时，静置分离， 得到富集天然玉米黄素的固体吸附剂;用 70°C的去离子水将富含天然玉米黄素的固体吸 附剂冲洗至所 pH为中性， 除去水；
固体吸附剂中加入乙酸乙酯 100毫升缓慢震荡， 静置分离， 除去固体吸附剂， 所得 溶剂浓缩干燥得到天然玉米黄素产品 5克， 通过与实施例 1相同的方法： 质谱、核磁共 振氢谱、 液相色谱等证明所得产物为玉米黄素， 纯度为 16%。

Claims

权利要求书
1、 一种原位富集法制备天然玉米黄素的制备方法， 其特征在于：
1 )将植物中的一种或二种以上部位干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg:10~100ml的比例加入提取溶剂， 30~80°C搅拌提取 1~10小时，提取结束后静置沉淀 过滤分离； 得提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 2-4 次；
3)合并提取液减压浓缩至溶剂蒸发完， 加入体积为原单次提取溶剂体积的 1/10 1 倍、 质量浓度 1~50%KOH或 NaOH的醇溶液， 10~80°C搅拌皂化 1~40小时；
4)皂化结束后加入固体吸附剂， 缓慢搅拌 0.5~10小时， 静置分离， 得到富集天然 玉米黄素的固体吸附剂； 用 20~60°C的去离子水或醇溶液将富含天然玉米黄素的固体吸 附剂冲洗至所 pH为中性， 除去溶液；
5) 固体吸附剂中加入中等极性溶剂缓慢震荡， 静置分离， 除去固体吸附剂， 所得 溶剂浓缩干燥得到天然玉米黄素产品。
2、 按照权利要求 1所述的制备方法， 其特征在于- 所述步骤 2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣再次进行提取， 提取 共重复 2-4次；
再次进行提取过程： 是指将上一步骤所得滤渣再次按照原料质量:溶剂体积 =lg:10~100ml的比例加入上述溶剂进行再次提取， 30~80°C搅拌提取 1~10小时，提取结 束后静置沉淀过滤分离； 得提取液和滤渣。
3、 按照权利要求 1所述的制备方法， 其特征在于： 所述植物是指植物的果实、 宿 萼、 根、 茎、 叶、 花或整个植株中的一种或二种以上； 所使用的植物为枸杞、 锦灯笼、 玉米、 辣椒、 沙棘、 南瓜、 柿子中的一种或二种以上。
4、 按照权利要求 1所述的制备方法， 其特征在于：
所述提取溶剂为： 甲醇、 乙醇、 丙醇、 丁醇、 乙酸乙酯、 二氯甲烷、 三氯甲烷、 乙 醚、 丙酮、 环己烷、 正己烷、 石油醚中的一种或二种以上的溶剂混合物；
所述中等极性溶剂为： 甲醇、乙醇、丙醇、丁醇、乙酸乙酯、二氯甲烷、三氯甲烷、 乙醚、 丙酮中的一种或二种以上；
所述固体吸附剂为： 二氧化硅、羟丙基葡聚糖凝胶、 聚苯乙烯树脂中的一种或二种 以上。
5、 按照权利要求 1所述的制备方法， 其特征在于：
步骤 3 )和 4) 中的醇溶液中的醇为甲醇、 乙醇、 丙二醇中的一种或二种以上。
6、 按照权利要求 1所述的制备方法， 其特征在于- 皂化结束后加入固体吸附剂的量为， 原料质量： 固体吸附剂质量 =1:0.1~10。
7、 按照权利要求 1所述的制备方法， 其特征在于：
中等极性溶剂的加入量为， 固体吸附剂质量： 中等极性溶剂体积 =lg:2~20ml。
8、 按照权利要求 1所述的制备方法， 其特征在于：
1 ) 将植物中的一种或二种以上干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg:10~50ml的比例加入提取溶剂， 30~60°C搅拌提取 1~10小时， 提取结束后静置沉淀 过滤分离； 得提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 2-4 次；
3)合并提取液减压浓缩至溶剂蒸发完， 加入体积为原提取溶剂体积的 1/2~1 倍、 质量浓度 5~30%KOH或 NaOH的醇溶液， 10~60°C搅拌皂化 1~40小时；
4)皂化结束后加入固体吸附剂， 固体吸附剂的加入量为， 原料质量： 固体吸附剂 质量 =1:0.5~8；缓慢搅拌 0.5~10小时，静置分离，得到富集天然玉米黄素的固体吸附剂； 用 20~50°C的去离子水或醇溶液将富含天然玉米黄素的固体吸附剂冲洗至所 pH为中性， 除去溶液；
5)固体吸附剂中加入中等极性溶剂，中等极性溶剂的加入量为：固体吸附剂质量- 中等极性溶剂体积 =lg:2~8ml; 缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓缩 干燥得到天然玉米黄素产品。
9、 按照权利要求 1所述的制备方法， 其特征在于：
1 ) 将植物中的一种或二种以上干燥后磨碎作为原料， 按照原料质量：溶剂体积 =lg:20ml的比例加入提取溶剂， 40°C搅拌提取 2小时， 提取结束后静置沉淀过滤分离; 得提取液和滤渣；
2)按照步骤 1 ) 的操作过程， 将上一步骤所得滤渣进行再次提取， 提取共重复 3 次；
3 )合并提取液减压浓缩至溶剂蒸发完， 加入体积为原提取溶剂体积的 1倍、 质量 浓度 10%KOH或 NaOH的醇溶液， 40°C搅拌皂化 10小时；
4)皂化结束后加入固体吸附剂， 固体吸附剂的加入量为， 原料质量： 固体吸附剂 质量 =1: 1 ; 缓慢搅拌 2小时，静置分离， 得到富集天然玉米黄素的固体吸附剂； 用 40°C 的去离子水或醇溶液将富含天然玉米黄素的固体吸附剂冲洗至所 pH为中性，除去溶液; 5) 固体吸附剂中加入中等极性溶剂， 中等极性溶剂的加入量为： 固体吸附剂质量： 中 等极性溶剂体积 =lg: 6ml; 缓慢震荡， 静置分离， 除去固体吸附剂， 所得溶剂浓缩干燥 得到天然玉米黄素产品。
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