WO2022021107A1 - 谷维素的制备方法 - Google Patents

谷维素的制备方法 Download PDF

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WO2022021107A1
WO2022021107A1 PCT/CN2020/105347 CN2020105347W WO2022021107A1 WO 2022021107 A1 WO2022021107 A1 WO 2022021107A1 CN 2020105347 W CN2020105347 W CN 2020105347W WO 2022021107 A1 WO2022021107 A1 WO 2022021107A1
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oryzanol
preparation
rice
solution
precipitate
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PCT/CN2020/105347
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English (en)
French (fr)
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陈瑞惠
詹育欣
高艾玲
陈劲中
蔡昌廷
蔡承佳
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台湾中油股份有限公司
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Priority to PCT/CN2020/105347 priority Critical patent/WO2022021107A1/zh
Priority to US17/429,510 priority patent/US20220162258A1/en
Publication of WO2022021107A1 publication Critical patent/WO2022021107A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07J—STEROIDS
    • C07J53/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by condensation with a carbocyclic rings or by formation of an additional ring by means of a direct link between two ring carbon atoms, including carboxyclic rings fused to the cyclopenta(a)hydrophenanthrene skeleton are included in this class
    • C07J53/002—Carbocyclic rings fused
    • C07J53/004—3 membered carbocyclic rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07J—STEROIDS
    • C07J53/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by condensation with a carbocyclic rings or by formation of an additional ring by means of a direct link between two ring carbon atoms, including carboxyclic rings fused to the cyclopenta(a)hydrophenanthrene skeleton are included in this class
    • C07J53/002—Carbocyclic rings fused
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils

Definitions

  • the present application relates to a preparation method of oryzanol, especially refers to a preparation method of oryzanol purified by supercritical fluid extraction.
  • Oryzanol ( ⁇ -oryzanol) is a compound formed by esterification of phytosterols, triterpenoids and ferulic acid. At present, it is known that oryzanol has the functions of inhibiting free radicals and anti-oxidation, and has the functions of reducing hyperlipidemia and alleviating menopausal discomfort.
  • oryzanol has been widely used in food and cosmeceutical products.
  • oryzanol is added to food to reduce the production of cholesterol oxides (COPs) in food; oryzanol is added to cream to promote cell growth.
  • COPs cholesterol oxides
  • Oryzanol is mainly extracted from vegetable oils.
  • Rice bran crude oil is the oil with the highest oryzanol content in vegetable oils.
  • Rice bran crude oil contains 1.4% to 2.9% of oryzanol. Therefore, rice bran crude oil is currently the commonly used raw material for oryzanol preparation.
  • oryzanol is also contained in other vegetable oils, such as corn oil, soybean oil, etc., which can also be used in the preparation of oryzanol.
  • the way to prepare oryzanol from rice bran crude oil is soapstock purification method. More specifically, in the process of refining rice bran crude oil into refined oil products, it includes steps such as degumming, deacidification, dewaxing, decolorization and deodorization. Alkali neutralizes its acidity, and during the deacidification process, a precipitate soapstock is obtained, and the soapstock can be used for further preparation of oryzanol.
  • the preparation process of the soapstock purification method includes: (a) homogenization: stirring the soapstock containing 60-70% of water at 70-90° C.
  • the purpose of this application is to address the above-mentioned problems, provide a kind of preparation method of high-purity oryzanol, and it comprises the following steps: (a) with supercritical fluid from the raw material containing oryzanol, extract the oryzanol-containing extract; (b) by the described Separating the oryzanol-containing precipitate from the oryzanol-containing extract by means of solid-liquid separation; and (c) purifying the oryzanol from the oryzanol-containing precipitate.
  • the oryzanol-containing raw material is selected from the group consisting of rice, wheat, corn, flaxseed and rapeseed.
  • the rice is selected from the group consisting of whole rice, brown rice after removing the husk, rice bran or white rice after the bran layer is removed, and the above-mentioned raw materials can be individually Or mixed and poured into the supercritical extraction tank.
  • the extraction temperature of the supercritical fluid is 30°C to 90°C, and the extraction pressure is 75 bar to 1000 bar.
  • step a the temperature of the oryzanol-containing extract is maintained at 60-80°C.
  • step b first filter out the oryzanol-containing filter residue from the oryzanol-containing extract, dissolve the oryzanol-containing filter residue in a non-polar solvent to form a solution to be separated, and then remove the oryzanol-containing filter residue from the to-be-separated solution.
  • the oryzanol-containing precipitate is separated from the separation solution.
  • the above preparation method in step c, is to dissolve the oryzanol in the oryzanol-containing precipitate in an organic solvent to form an oryzanol purified solution, then filter the oryzanol purified solution to form an oryzanol purified filtrate, and the oryzanol The oryzanol is obtained by removing the organic solvent in the purified filtrate.
  • the oryzanol purified solution is heated to 35-40° C. before filtration.
  • Fig. 1 is the flow chart of the preparation method of oryzanol of the embodiment of the application.
  • the preparation method of oryzanol in the present embodiment comprises the following steps: (a) extracting an oryzanol-containing extract from the oryzanol-containing raw material with supercritical fluid; (b) extracting an oryzanol-containing extract from the oryzanol-containing extract; The oryzanol-containing precipitate is separated by liquid separation; and (c) oryzanol is purified from the oryzanol-containing precipitate.
  • Oryzanol-containing extract is extracted from oryzanol-containing raw materials:
  • the temperature of the oryzanol-containing extract can be maintained at 80°C through an oven, so that the oryzanol-containing extract can be maintained at a fluid level. Dark brown oily state, but the oryzanol-containing extract can also be maintained at other temperature ranges that can be kept in a fluid state, for example, between 60 and 80 °C, as required.
  • the vaporized carbon dioxide can be re-pressurized into liquid carbon dioxide as a supercritical fluid, reused and stored in the circulating pipeline.
  • water, ethanol or other currently known suitable supercritical fluid materials can be used as the co-solvent of carbon dioxide, and other suitable fluid types can also be selected, and the extraction temperature can be adjusted according to the process requirements or the properties of the supercritical fluid. It is set at 30-90 °C, and the extraction pressure is set at about 75-1000 bar, but the temperature and pressure can still be set in other numerical ranges depending on the process requirements or the properties of the supercritical fluid, not limited to the above.
  • the oryzanol-containing raw material can be rice, brown rice, white rice, rice bran or a mixture thereof, but also wheat, corn, or plant raw materials with high oil content such as flaxseed and rapeseed.
  • the oryzanol-containing precipitate is separated from the oryzanol-containing extract by solid-liquid separation:
  • the oryzanol-containing extract is subjected to solid-liquid separation.
  • the oryzanol-containing extract is first filtered with filter paper, and the dark brown filtrate and the off-white filter residue are separated, and the off-white filter residue contains oryzanol.
  • the oryzanol-containing precipitate is separated from the solution to be separated by centrifugation, but filtration or other known solid-liquid separation methods can also be used to separate the oryzanol-containing precipitate.
  • the aforementioned n-hexane supernatant can be recovered and used again after distillation under reduced pressure.
  • the precipitate left after the filter residue is washed with n-hexane can be placed in a chemical extraction cabinet to dry naturally, so that the n-hexane in the precipitate can be completely volatilized, or the n-hexane in the precipitate can be extracted by vacuum decompression to remove Residual n-hexane in the precipitate.
  • n-hexane is selected as the non-polar solvent, but non-polar solvents with similar properties such as n-heptane, linear or cyclic hydrocarbon solvents can also be selected.
  • the steps of filtering the oryzanol-containing extract and cleaning the filter residue are simultaneously performed, but in other embodiments, only filtering can be performed.
  • the step of containing the oryzanol extract, and the filter residue is directly used as the oryzanol-containing precipitate for subsequent purification.
  • Oryzanol is purified from oryzanol-containing precipitates:
  • acetone is used to dissolve the oryzanol in the precipitate, that is, the oryzanol in the precipitate is dissolved in acetone.
  • a purified solution of oryzanol is formed thereby, and the dissolving situation of oryzanol is monitored by thin layer chromatography (TLC) until the oryzanol is no longer dissolved in the oryzanol-containing precipitate.
  • TLC thin layer chromatography
  • this step also Can be omitted.
  • the oryzanol purification solution is heated, then filter, thus obtain clear acetone filtrate as the oryzanol purification filtrate, the oryzanol purity obtained by the oryzanol purification filtrate is higher, but in other embodiments, also can omit filtering oryzanol purification as required solution steps.
  • the oryzanol purified filtrate is subjected to vacuum distillation to recover the acetone solution, and the oryzanol can be separated out while the acetone solution is recovered, or the oryzanol purified filtrate is placed in a low-temperature environment to separate out the oryzanol, and then solid-liquid separation is carried out at low temperature. to get oryzanol.
  • the precipitated oryzanol is in the form of powder. In order to further remove the residual solvent, the precipitated oryzanol can be placed in an oven and baked at 50° C. overnight.
  • acetone is used to dissolve oryzanol from the oryzanol-containing precipitate, but ethyl acetate, isopropanol, ethanol, methanol, a mixture thereof, or an organic solvent similar to its properties can also be selected.
  • the final sample powder prepared by the preparation method of this embodiment was qualitatively and quantitatively determined in the following ways.
  • headspace gas chromatography mass spectrometry (Headspace GC-MS) was used to measure the residual solvent in the sample powder, and the result of the measurement was that no solvent remained in the sample powder.
  • the moisture content of the sample powder was measured by the drying weight loss method, and the measured result was that the moisture in the sample powder accounted for 0.32% of the total weight by weight, indicating that the sample powder contained very little moisture.
  • the inorganic impurity content of the sample powder was determined by the residue-on-ignition method, and the inorganic impurity content of the sample powder accounted for 2.53% of the total weight, indicating that the sample powder contained very few inorganic impurities.
  • the microbiological quick sieve (3M Petrifilm AC, RYM, EC, STX and CompactDry PA) was used to detect the total number of bacteria and fungi in the sample powder, and to detect whether it contained Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa, after testing, no microorganisms were detected in the sample powder.
  • the solution to be tested has the maximum absorption at 229-233nm, 289-293nm and 313-317nm. Contains oryzanol.
  • the preparation method of the above-mentioned oryzanol can prepare high-purity oryzanol at room temperature, the obtained oryzanol has a purity of more than 95%, and the process steps are simple, and the homogenization, alkalization, The steps of saponification, dehydration, dissolution and the like solve the problem of complicated manufacturing process of the existing method for preparing oryzanol.
  • the above-mentioned preparation method of oryzanol produces less waste, and the solvent used in the above-mentioned preparation method of oryzanol can be recovered and reused by distillation.

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Abstract

一种谷维素的制备方法，包含下列步骤：（a）以超临界流体由含谷维素的原料中萃取出含谷维素萃取液；（b）由所述含谷维素萃取液中以固液分离方式分离出含谷维素沉淀物；及（c）由所述含谷维素沉淀物中纯化出谷维素。

Description

谷维素的制备方法 技术领域
本申请关于一种谷维素的制备方法，尤其是指一种通过超临界流体萃取纯化出谷维素的制备方法。
背景技术
谷维素(γ-oryzanol)为一种由植物固醇(phytosterols)、三萜类合物(triterpenoids)与阿魏酸(ferulic acid)酯化而成的化合物。目前已知谷维素具有抑制自由基及抗氧化的作用，并且具有降高血脂、减轻更年期不适等功效。
目前谷维素已广泛应用于食品、药妆产品中，例如，将谷维素添加于食品中来减少食品的胆固醇氧化物(cholesterol oxidation products,COPs)的生成；将谷维素添加到乳霜中，可用以促进细胞增生及增进皮肤弹性的保湿度。
谷维素主要萃取自植物油脂，米糠粗油为植物油脂中谷维素含量最高的油类，米糠粗油中含有1.4％～2.9％的谷维素，因此，米糠粗油为目前常用的谷维素制备原料。但在其它植物油中也含有谷维素，例如玉米油、大豆油等，也可应用于制备谷维素。
一般利用米糠粗油来制备谷维素的方式为皂脚纯化法。更具体而言，在将米糠粗油精炼成精炼油品的过程中，包含脱胶、脱酸、脱蜡、脱色及脱臭等步骤，在脱酸步骤中，通过将经粗油脱胶后的原油以碱中和其酸性，在此脱酸过程中会得到沉淀物皂脚，皂脚即可用于进一步制备谷维素。皂脚纯化法的制备过程包括：(a)均质：将含有水份60～70％的皂脚，以70～90℃、pH10～11的条件，搅拌均匀；(b)碱化：在皂脚中加入0.2～1.2％氢氧化钠，持续搅拌均匀；(c)皂化：将前述皂脚在70～90℃下持续搅拌约30～45分钟，得到皂化皂脚；(d)脱水：将前述的皂化皂脚进行脱水；(e)溶出：将脱水后的皂化皂脚用溶剂溶出；及(f)去除溶剂取得谷维素萃取液。
然而，如前所述，在以皂脚纯化法制备谷维素的制程中，至少需要经过均质、碱化、皂化、脱水、溶出等大量步骤，使得制备谷维素的制程相当复杂。
发明内容
本申请的目的即针对上述问题，提供一种高纯度谷维素的制备方法，其包含下列步骤：(a)以超临界流体由含谷维素的原料中萃取出含谷维素萃取液；(b)由所述含谷维素萃取液中以固液分离方式分离出含谷维素沉淀物；及(c)由所述含谷维素沉淀物中纯化出谷维素。
如上所述的制备方法，在步骤a中，所述含谷维素原料选自由稻类、麦类、玉米、亚麻籽及油菜籽所组成的组。
如上所述的制备方法，当所述含谷维素原料选自稻类时，稻类选自由完整稻谷、去外壳后的糙米、米糠或去糠层后的白米所组成的组，且上述原料可以单独或混合倒入超临界萃取槽中。
如上所述的制备方法，在步骤a中，所述超临界流体的萃取温度为30℃至90℃，且萃取压力为75bar至1000bar。
如上所述的制备方法，在步骤a中，所述含谷维素萃取液的温度维持于60～80℃。
如上所述的制备方法，在步骤b中，先由所述含谷维素萃取液中过滤出含谷维素滤渣，将所述含谷维素滤渣溶于非极性溶剂中形成待分离溶液，再由所述待分离溶液中分离出所述含谷维素沉淀物。
如上所述的制备方法，在步骤c中，是使所述含谷维素沉淀物中的谷维素溶于有机溶剂中形成谷维素纯化溶液，再将所述谷维素纯化溶液过滤形成谷维素纯化滤液，将所述谷维素纯化滤液中的有机溶剂去除取得所述谷维素。
如上所述的制备方法，所述谷维素纯化溶液在过滤前加热至35～40℃。
经由如上所述的谷维素的制备方法，可以在常温状态下制备出高纯度谷 维素，并且制程步骤简单，由此解决现有制备谷维素的方法其制程复杂的问题。
附图说明
图1为本申请实施例的谷维素的制备方法流程图。
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具体实施方式
为了充分了解本申请的目的、特征及功效，通过下述具体的实施例，对本申请做一详细说明，说明如后：
参见图1，本实施例中的谷维素的制备方法包含下列步骤：(a)以超临界流体由含谷维素的原料中萃取出含谷维素萃取液；(b)由所述含谷维素萃取液中以固液分离方式分离出含谷维素沉淀物；及(c)由所述含谷维素沉淀物中纯化出谷维素。上述各步骤将于后续具体阐述。
由含谷维素的原料中萃取出含谷维素萃取液：
首先，以糙米作为原料，将约12吨的糙米充填于三个串连式的吨级萃取槽(各萃取槽的体积为6m3)，并以二氧化碳作为超临界流体，由糙米中萃取出油脂，萃取温度设定在大约50℃，萃取压力设定在约270bar，萃取时间为6～7小时，由糙米萃出的含谷维素萃取液为深褐色油脂，含谷维素萃取液中带有米白色混浊物，上述萃取制程进行8个批次，最终可得到200L糙米粗油。
为使含谷维素萃取液具有更佳的流动性以利于含谷维素萃取液后续的分离谷维素步骤，可通过烘箱使含谷维素萃取液的温度维持于80℃，使含谷维素萃取液维持在具流动性的深褐色油脂状态，但也可视需求将含谷维素萃取 液维持于可保持于流体状态的其他温度范围，例如，60～80℃之间。
在此萃取步骤中，气化的二氧化碳可以重新加压成液体二氧化碳作为超临界流体，在循环的管线中重复使用及储存。
在此萃取步骤中，可以水、乙醇或其他目前已知合适的超临界流体材料作为二氧化碳的共溶剂，也可以选择其他的适当流体种类，并且根据制程需求或超临界流体性质，可以将萃取温度设定在30～90℃，萃取压力设定在约75～1000bar，但仍可视制程需求或超临界流体性质将温度和压力设定在其他数值范围，不以上述为限。
在此萃取步骤中，含谷维素原料可以是稻谷、糙米、白米、米糠或其混合物，但也可选用麦类、玉米，或是亚麻籽、油菜籽等油脂含量高的植物原料。
此外，在进行超临界流体萃取过程中，为提高萃取率，可以添加例如乙醇等现有已知的共溶剂。
由所述含谷维素萃取液中以固液分离方式分离出含谷维素沉淀物：
首先，将含谷维素萃取液进行固液分离，在本实施例中，先将含谷维素萃取液以滤纸进行过滤，分离出深褐色滤液及米白色滤渣，米白色滤渣中含有谷维素。接着，清洗滤渣，将滤渣溶于非极性溶剂正己烷中形成待分离溶液，再将待分离溶液进行离心得到含谷维素的沉淀物(pellet)及上清液，上清液若呈淡黄色，则再次加入新的正己烷清洗沉淀物，如此以正己烷反复清洗滤渣，直到将待分离溶液进行离心后得到的上清液呈无色，此时表示以肉眼已经看不到沉淀物中的杂质溶入正己烷，含谷维素滤渣被充分清洗。
在本实施例中，是通过离心从待分离溶液中分离出含谷维素的沉淀物，但也可选用过滤或是现有已知的其他固液分离方法分离出含谷维素的沉淀物。
前述的正己烷上清液可经由减压蒸馏后再次回收使用。滤渣经过正己烷清洗后留下的沉淀物可置于化学抽气柜中自然风干，让沉淀物中的正己烷完 全挥发，或是通过真空减压抽气抽取沉淀物中的正己烷，以去除沉淀物中残留的正己烷。
在本实施例中，是选用正己烷作为非极性溶剂，但也可选用正庚烷、直链或环状的碳氢化合物溶剂等性质相近的非极性溶剂。
在本实施例中，为充分去除含谷维素沉淀物中的杂质，以利后续纯化谷维素，因此，同时进行过滤含谷维素萃取液及清洗滤渣的步骤，但在其他实施例中，也可仅进行过滤含谷维素萃取液的步骤，并以滤渣直接作为后续纯化之用的含谷维素沉淀物。
由含谷维素沉淀物纯化出谷维素：
由于前述含谷维素沉淀物含有杂质、碎屑等不可溶物，为取得高纯度谷维素，在此步骤中，是利用丙酮将沉淀物中的谷维素溶出，也即，使沉淀物中的谷维素溶于丙酮中，由此形成谷维素纯化溶液，以薄层层析技术(Thin layer chromatography,TLC)监测谷维素的溶解情形，直到含谷维素沉淀物中不再溶出谷维素为止。接着，将前述谷维素纯化溶液预先加热维持于35～40℃，避免在过滤时因谷维素纯化溶液的温度下降造成谷维素提前析出，进而使后续回收的谷维素量减少，但在其他实施例，此步骤也可省略。待谷维素纯化溶液加热完成后，接着进行过滤，由此获得澄清丙酮滤液作为谷维素纯化滤液，由谷维素纯化滤液所得到的谷维素纯度更高，但在其他实施例中，也可视需求省略过滤谷维素纯化溶液的步骤。最后，将谷维素纯化滤液进行减压蒸馏以回收丙酮溶液，在回收丙酮溶液的同时便可将谷维素析出，或是将谷维素纯化滤液放置于低温环境中使谷维素析出，再于低温下进行固液分离来取得谷维素。析出的谷维素呈粉末状，为了进一步移除残留的溶剂，可以将析出的谷维素放置于烘箱中以50℃烘烤过夜。
在本实施例中，是选用丙酮从含谷维素沉淀物中溶出谷维素，但也可选用乙酸乙酯、异丙醇、乙醇、甲醇、其混合物或与其性质相近的有机溶剂。
谷维素定性及定量测定：
为测定以前述制备方法所制得的谷维素的纯度，以下列几种方式对由本实施例的制备方法所制得的最终样品粉末进行定性及定量测定。
氢氧化钾-乙醇呈色定性测定法：
取0.01g的样品粉末溶于10mL的氢氧化钾-乙醇溶液中(10％,w/v)，若溶液呈现黄色，即代表溶液中有谷维素，测得结果为溶液呈现黄色。
氯化铁呈色定性测定法：
取0.01g的样品粉末溶于2mL的丙酮溶液中，再加入0.1mL氯化铁乙醇(2％,w/v)，若溶液呈现黄绿色或绿色，即代表溶液中有谷维素，测得结果为溶液呈现黄绿色。
残留溶剂：
在本实施例中，采用顶空气相层析质谱法(Headspace GC-MS)测定样品粉末中的残留溶剂，测得结果为样品粉末中并无溶剂残留。
含水量测定：
在本实施例中，采用干燥减重法测定样品粉末含水量，测得结果为样品粉末中的水分占总重的重量百分比为0.32％，表示样品粉末中的水分极少。
无机杂质含量测定：
在本实施例中，采用炽灼残渣测定法测定样品粉末的无机杂质含量，样品粉末的无机杂质占总重的重量百分比为2.53％，表示样品粉末中的无机杂质极少。
重金属含量测定：
在本实施例中，参考卫生福利部食品药物管理署所公布的“化妆品中铅、镉及砷鉴别及含量测定方法”以及“化妆品中汞鉴别及含量测定方法”，利用电感耦合等离子体质谱(ICP-MS)检测样品粉末中是否含有重金属，测得结果为样品粉末中并未检测出铅(Pb)、砷(As)、镉(Cd)、汞(Hg)等重金属物质。
微生物含量测定：
在本实施例中，以微生物快筛片(3M Petrifilm AC、RYM、EC、STX及 CompactDry PA)，检测样品粉末中的总生菌数及真菌数，并检测是否含有大肠杆菌、金黄色葡萄球菌及绿脓杆菌，经检测后，样品粉末中并未检测出含有微生物。
谷维素纯度测定：
首先，取0.025g的样品粉末，将其置于5mL定量瓶中，加入0.5mL丙酮使样品粉末溶解，再加入正庚烷到前述5mL定量瓶中将溶液体积补至5mL，制成预处理溶液。另取25ml定量瓶，将正庚烷倒入前述25ml定量瓶中达九分满，再加入50μL的预处理溶液到前述25ml定量瓶中，并以正庚烷将溶液体积补至25mL，制成待测溶液。使用分光光度计以OD315的条件测定待测溶液的吸光值。并以下列公式计算谷维素含量。带入公式:谷维素含量(％)＝(A×2500)/(W*E)(W＝样品重量g；A＝样品315nm吸光值；E＝吸收系数1％(光径1cm)＝359)。最后测得样品粉末中的谷维素含量达>95％，证明由本实施例的制备方法所制得的谷维素其纯度可达95％以上。
此外，当将前述待测溶液以其他波长测定其吸光值时，前述待测溶液在229-233nm、289-293nm及313-317nm有最大吸收量，此吸光值范围分布也可证明待测溶液中含有谷维素成分。
上述谷维素的制备方法，可以在常温状态下制备出高纯度谷维素，所制得的谷维素纯度可达95％以上，并且制程步骤简单，可省去皂脚纯化法所需的均质、碱化、皂化、脱水、溶出等步骤，由此解决现有制备谷维素的方法其制程复杂的问题。此外，上述谷维素的制备方法相较于现有皂脚纯化法，其所产生的废弃物较少，上述谷维素的制备方法于制程中使用的溶剂均可蒸馏回收再利用。
虽然已经出于说明性目的描述了各种实施例，但是对于本领域技术人员来说显而易见的是，在不脱离如所附权利要求中所限定的本申请的精神和范围的情况下，可以进行各种改变和改进。

Claims (8)

  1. 一种谷维素的制备方法，其特征在于，包含下列步骤：
    (a)以超临界流体由含谷维素的原料中萃取出含谷维素萃取液；
    (b)由所述含谷维素萃取液中以固液分离方式分离出含谷维素沉淀物；及
    (c)由所述含谷维素沉淀物中纯化出谷维素。
  2. 根据权利要求1所述的制备方法，其特征在于，在步骤a中，所述含谷维素原料选自由稻类、麦类、玉米、亚麻籽及油菜籽所组成的组。
  3. 根据权利要求2所述的制备方法，其特征在于，当所述含谷维素原料选自稻类时，稻类选自由完整稻谷、去外壳后的糙米、米糠或去糠层后的白米所组成的组。
  4. 根据权利要求1所述的制备方法，其特征在于，在步骤a中，所述超临界流体的萃取温度为30℃至90℃，且萃取压力为75bar至1000bar。
  5. 根据权利要求1所述的制备方法，其特征在于，在步骤b中，所述含谷维素萃取液在固液分离前使其温度维持于60～80℃。
  6. 根据权利要求1所述的制备方法，其特征在于，在步骤b中，先由所述含谷维素萃取液中过滤出含谷维素滤渣，将所述含谷维素滤渣溶于非极性溶剂中形成待分离溶液，再由所述待分离溶液中分离出所述含谷维素沉淀物。
  7. 根据权利要求1所述的制备方法，其特征在于，在步骤c中，是使含谷维素沉淀物中的谷维素溶于有机溶剂中形成谷维素纯化溶液，再将所述谷维素纯化溶液过滤形成谷维素纯化滤液，将所述谷维素纯化滤液中的有机溶剂去除取得所述谷维素。
  8. 根据权利要求7所述的制备方法，其特征在于，所述谷维素纯化溶液在过滤前加热至35～40℃。
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