WO2019100538A1 - 一种火麻油的提取工艺 - Google Patents

一种火麻油的提取工艺 Download PDF

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Publication number
WO2019100538A1
WO2019100538A1 PCT/CN2018/000041 CN2018000041W WO2019100538A1 WO 2019100538 A1 WO2019100538 A1 WO 2019100538A1 CN 2018000041 W CN2018000041 W CN 2018000041W WO 2019100538 A1 WO2019100538 A1 WO 2019100538A1
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oil
water
sesame oil
hemp
extracting
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PCT/CN2018/000041
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English (en)
French (fr)
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陈程
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陈程
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    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • 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
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter

Definitions

  • the invention belongs to the technical field of vegetable oil extraction, and particularly designs an extraction process of fire oil.
  • Hemp oil traditionally known as longevity hemp, longevity oil, extracted from hemp, has a very high nutritional value.
  • the food has the effects of moistening the intestines, nourishing yin and nourishing, helping digestion, improving eyesight and protecting liver, rickets and longevity, and has special curative effect on diseases such as constipation, high blood pressure and high cholesterol, and hemp is the only one that is soluble in water. Oil.
  • the existing preparation process of the hemp pressure oil is usually obtained by drying, crushing and high-temperature steaming and then high-temperature pressing, and the nutrients are excessively lost due to excessive temperature and the like.
  • Invention patent CN200710195010.5 A process for processing hemp oil, which is based on hemp seed, after water removal, screening, peeling, drying, quenching and tempering, pressing, oil treatment and cold-squeezed tablet pressing section , obtained cold-refined refined hemp kernel oil.
  • the invention avoids the use of the extraction method to introduce the chemical solvent to obtain the oil and fat, and the oil quality is affected by the existence of the residual solution; and the oil absorption caused by the scum of the hemp seed shell in the cold pressed embryo sheet is avoided.
  • the press roll is not easily pressed and the like, thereby improving the yield of the extract of the hemp oil from the hemp seed.
  • Invention patent CN201210127891.8 A method for ultrasonically assisting supercritical CO 2 extraction of sesame oil, comprising the following steps: (1) pretreatment to remove impurities in hemp kernel, and then the water content in the roasted hemp kernels is reduced to 10% Hereinafter, mechanical pulverization, sieving and grading; (2) weighing the hemp seed powder treated in the step (1), adding the anti-caking agent and mixing uniformly; (3) placing the hemp seed powder processed in the step (2) into the super
  • the extraction tank in the critical extraction device is equipped with an ultrasonic generating device, and then extracted to obtain hemp oil.
  • the invention extraction ultrasonic extraction combined extracted by supercritical CO with, and adding an anti-caking agent, under the same extraction conditions, adding an anti-caking agent and ultrasonic assisted ultra-extracted with supercritical CO may be original simple supercritical CO extraction efficiency 2 Increasing the 3-4%, significantly improving the supercritical extraction efficiency, is a simple, efficient and safe method for extracting sesame oil.
  • the present invention provides a process for extracting castor oil at a low temperature.
  • a method for extracting sesame oil comprising the following steps:
  • reaction solution is centrifuged at 3000 r/min for 20 to 50 minutes to obtain oil phase I, aqueous phase I, emulsion and precipitation;
  • the main active ingredients of Hemp seed include fatty acids and lipids, lignans, amides, steroids, cannabinoids, flavonoids and glycosides, alkaloids, volatile oils, proteins and amino acids, vitamins and trace elements.
  • the small amount of water contained in the sesame oil will combine with the lipids, and the solubility in the oil will decrease, affecting the flavor of the oil; the vitamin B group rich in grape juice is mainly inositol substances, inositol and sesame oil.
  • Phospholipids can react to produce phytic acid; phytic acid has strong antioxidant activity, enhances the anti-oxidation effect of sesame oil, and also inhibits the production of aflatoxin with strong carcinogenic effects; at the same time, phytic acid can promote body fat metabolism and reduce Blood lipids, inhibit the production of cholesterol, improve the health value of sesame oil.
  • the Maillard reaction occurs with the sesame oil at high temperature to improve the flavor of the sesame oil and promote the flavor of the sesame oil.
  • the ginger protease can promote the oil yield of the sesame oil and improve the oil yield. The oil extraction rate of the sesame oil in the first extraction of the residue.
  • the inositol in the grape juice and the phospholipids in the hemp can maximize the synthesis of phytic acid and further increase the phytic acid content of the sesame oil.
  • the pulverized hemp seed powder according to the step (2) has an average particle diameter of 180 to 200 mesh.
  • the grape juice preparation method in the step (3) is: taking fresh and disease-free grapes for juice extraction, taking the supernatant after centrifugation filtration, and diluting to 10 to 20 times with water.
  • the demulsification rate in the step (5) is 93 to 94%.
  • the preparation method of the ginger extract in the step (6) is as follows:
  • the ginger is washed, peeled and dried, it is cut into 1-2 mm slices, extracted with absolute ethanol at a ratio of 1:6 in a constant temperature water bath at 50 ° C for 4 h, filtered, and the filtrate is concentrated to dryness by vacuum rotary evaporation. Then, it was dissolved in 100 mL of water, an equal volume of ethyl acetate was added, and the mixture was extracted three times. The ethyl acetate layer was combined and concentrated by vacuum evaporation to obtain a ginger extract.
  • the content of each substance in the total alkaloid adsorption solution of the Coptidis Rhizoma described in the step (7) is: palmatine 11-13 mg/ml, small chopping wood 34-36 mg/ml, and coptisine 20. 22 mg/ml.
  • the preparation method of the supported total alkaloid adsorption solution of Coptidis Rhizoma described in the step (7) is as follows:
  • the activated carbon fiber material was taken, and the total alkaloid solution of Rhizoma Coptidis was added, and the adsorption solution was stirred at a water temperature of 40 ° C for 90 min to prepare an adsorption solution containing 80-120 ml/g of total alkaloids of Coptidis Rhizoma.
  • Activated carbon fiber has large specific surface area and micropore volume, and has large adsorption capacity and fast adsorption speed. Therefore, activated carbon fiber loaded with berberine alkaloid can rapidly adsorb benzo( ⁇ ) oxime in castor oil; activated carbon fiber is insoluble in oil. Easy to centrifuge.
  • the preparation process of the invention is simple, the raw materials are simple to obtain, all are natural plant materials, the cost is low and the toxic substances are low, and the reaction conditions of each process are easy to control;
  • the present invention utilizes grape juice, ginger and berberine which are of health value to the human body to assist the extraction of sesame oil, not only improves the extraction rate of sesame oil, but also increases the scent of sesame oil, and at the same time improves the health value of sesame oil.
  • the preparation method of the grape juice is: taking fresh and disease-free grapes for juice extraction, taking the supernatant after centrifugation filtration, and diluting to 10 times with water;
  • reaction solution was centrifuged at 3000 r/min for 20 min to obtain oil phase I, aqueous phase I, emulsion and precipitation;
  • the preparation method of the ginger extract is as follows: after the ginger is washed, peeled, and dried, it is cut into a sheet of 1 to 2 mm, and the absolute ratio of the liquid to liquid is 1:50 (m/v) at 50 ° C. The mixture was extracted in a water bath for 4h, filtered, and the filtrate was concentrated to dryness by vacuum rotary evaporation, then dissolved in 100 mL of water, and then added with an equal volume of ethyl acetate, extracted three times, and the ethyl acetate layer was combined and concentrated by vacuum evaporation to obtain a ginger extract;
  • the content of each substance in the total alkaloid adsorption solution of Coptidis Rhizoma is 11% for palmatine, 34% for small chopped wood, and 20% for berberine;
  • the preparation method is as follows: the activated carbon fiber material is taken, the berberine alkaloid solution is added, and the adsorption is carried out for 90 min at 40 ° C water temperature to prepare a 80 mg/g loaded total aqueous alkaloid adsorption solution of Coptidis Rhizoma.
  • the preparation method of the grape juice is: taking fresh and disease-free grapes for juice extraction, taking the supernatant after centrifugation filtration, and diluting to 20 times with water;
  • reaction solution was centrifuged at 3000 r/min for 50 min to obtain oil phase I, aqueous phase I, emulsion and precipitation;
  • the preparation method of the ginger extract is as follows: after the ginger is washed, peeled, and dried, it is cut into a sheet of 1 to 2 mm, and the absolute ratio of the liquid to liquid is 1:50 (m/v) at 50 ° C. The mixture was extracted in a water bath for 4h, filtered, and the filtrate was concentrated to dryness by vacuum rotary evaporation, then dissolved in 100 mL of water, and then added with an equal volume of ethyl acetate, extracted three times, and the ethyl acetate layer was combined and concentrated by vacuum evaporation to obtain a ginger extract;
  • the content of each substance in the total alkaloid adsorption solution of Coptidis Rhizoma is 13% for palmatine, 36% for small chopped wood, and 22% for berberine;
  • the preparation method is as follows: the activated carbon fiber material is taken, the berberine alkaloid solution is added, and the adsorption is carried out for 90 min at 40 ° C water temperature to prepare a 120 mg/g supported total alkaloid adsorption solution of Coptidis Rhizoma.
  • the extraction rate of the sesame oil was 36.9%.
  • the preparation method of the grape juice is: taking fresh and disease-free grapes for juice extraction, taking the supernatant after centrifugation filtration, and diluting to 12 times with water;
  • reaction solution was centrifuged at 3000 r/min for 40 min to obtain oil phase I, aqueous phase I, emulsion and precipitation;
  • the preparation method of the ginger extract is as follows: after the ginger is washed, peeled, and dried, it is cut into a sheet of 1 to 2 mm, and the absolute ratio of the liquid to liquid is 1:50 (m/v) at 50 ° C. The mixture was extracted in a water bath for 4h, filtered, and the filtrate was concentrated to dryness by vacuum rotary evaporation, then dissolved in 100 mL of water, and then added with an equal volume of ethyl acetate, extracted three times, and the ethyl acetate layer was combined and concentrated by vacuum evaporation to obtain a ginger extract;
  • the content of each substance in the total alkaloid adsorption solution of Coptidis Rhizoma is 12% for palmatine, 35% for small chopped wood, and 21% for berberine;
  • the preparation method is as follows: the activated carbon fiber material is taken, the berberine alkaloid solution is added, and the adsorption is carried out for 90 min at 40 ° C water temperature to prepare a 110 mg/g supported total alkaloid adsorption solution of Coptidis Rhizoma.
  • the extraction rate of the sesame oil in this example was 37.2%.
  • Ultrasonic-assisted supercritical CO 2 extraction of sesame oil which comprises the following steps:
  • the oil extraction rate in the comparative example is low, and the equipment is required to be high and the cost is high.
  • the fire oil prepared in Examples 1 to 3 and the fire oil prepared in the comparative example were subjected to an edible test, and 50 experimenters were randomly selected, and each of the men and women was allowed to use the examples to obtain the sesame oil and the comparative example system.
  • the sesame oil was obtained for 10 days, and then the sensory tastes of the two sesame oils were scored, out of 5, the higher the score, the better the sensory taste, and the average score was summarized in Table 1.

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Abstract

一种火麻油的提取工艺，利用葡萄汁中的肌醇去除榨油中产生的磷脂，降低火麻油提取过程中磷脂含量，降低了干燥工艺含水量的要求；肌醇能与磷脂反应生成植酸，提高了火麻油的品质与营养价值；再利用生姜与提取工段副产物反应，生成更多的香味物质吡嗪，与火麻油混合加热后，提高火麻油的香味。该方法中的原料均是市场易于购买的物质，提取工艺简单，不含有化学试剂，制备得到的火麻油风味好，香气足，具有很好的发展前景。

Description

一种火麻油的提取工艺 技术领域
本发明属于植物油提取技术领域，特别设计一种火麻油的提取工艺。
背景技术
火麻油，传统习惯称之为长寿麻、长寿油，从火麻中榨取获得，有极高的营养价值。食之有润肠胃、滋阴补虚、助消化、明目保肝、祛病益寿之功效，且对便秘、高血压和高胆固醇等疾病有特殊的疗效，而且火麻是唯一能够溶于水的油料。现有火麻压油制备工艺，通常先进行烘干、破碎和高温蒸抄后进行高温压榨制备而得，由于温度过高等原因导致营养成分过度流失。
发明专利CN200710195010.5一种火麻油脂加工工艺，该油脂是以火麻籽为原料，经除水、筛选清理、脱皮、烘干、调质、压榨、油处理和冷榨胚片压榨工段后，获得冷榨精制火麻仁油脂。该发明避免了使用萃取法引入化学溶剂来获取油脂，而由于残溶的存在而给油脂品质带来影响；避免了因冷榨胚片中含有火麻籽壳碎渣所带来的诸如吸油，压榨辊不易压紧等不利影响，从而提高从火麻仁中提取火麻油脂的产率。发明专利CN201210127891.8一种超声波辅助超临界CO 2萃取火麻油的方法，包括如下步骤：(1)预处理去除火麻仁中的杂质，然后烘烤火麻仁中的含水量降至10％以下，机械粉碎、过筛分级；(2)称取步骤(1)处理的火麻仁粉，加入抗结剂并混合均匀；(3)将步骤(2)处理的火麻仁粉置入超临界提取设备中的提取罐中，并加装超声波发生装置，然后进行提取得到火麻油。该发明提取技术将超声波提取与超临界CO 2萃取相结合，并加入抗结剂，相同萃取条件下，加入抗结剂并以超声波辅助超临界CO 2萃取可将原来单纯超临界CO 2萃取效率提高3～4％，显著提高了超临界的萃取效率，是一种提取火麻油的简单、高效、安全的方法。
现有技术中，对植物油的提取主要集中于机械压榨，其中热榨法出油率高且产品风味极佳，但品质差；冷榨法可以较好的保护营养成分，但是存在缺乏香味，残油率较高的问题。
发明内容
针对现有技术中火麻油提取过程中由于温度过高导致营养成分过度流失，本发明提供一种低温提取火麻油的工艺。
本发明是通过以下技术方案实现的：
一种火麻油的提取工艺，包括以下步骤：
(1)去除火麻仁的杂质，然后烘烤火麻仁使含水量降至7～12％，然后对烘干后的火麻仁进行脱皮；将脱皮后的火麻仁采用刀片式中药粉碎机进行粉碎，得到火麻仁粉；
(2)将火麻仁粉与葡萄汁按料液比为1∶(1～5)混合均匀，调节pH为9～11，反应温度为70～80℃，浸提0.5～1.5h后得到反应液；所述液料比单位以g/mL计；
(4)将反应液于3000r/min下离心分离20～50min，得到油相I、水相I、乳状液和沉淀；
(5)取乳状液于-1～5℃下冷冻至凝结，然后将其置于35～40℃下放置破乳30～40min，8000r/min下离心15～20min，得到油相II和水相II；
(6)将水相I、水相II混合均匀，加热浓缩至原体积的10～20％，然后按料液比1∶(6～10)加入生姜浸膏混合均匀，于50～60℃下水水浴加热1.5～2h，得到水解液；所述液料比单位以g/mL计；
(7)将油相I和油相II混合均匀得到混合油，然后加入步骤(6)所得水解液，再加入混合油体积5～10％的负载黄连总生物碱吸附溶液，混合均匀后转入高压反应釜中，加热升温到110～170℃后保温10～20min，然后冷却至室温，离心分离去除水相和杂质，即可得到火麻油。
火麻仁的主要活性成分包括脂肪酸和脂类、木脂素、酰胺类、甾体类、***酚类、黄酮和苷类、生物碱、挥发油、蛋白质和氨基酸、维生素和微量元素等，在提油过程中，火麻油含有的少量水分会和脂类结合，在油中溶解度降低，影响油的风味；葡萄汁中富含的维生素B族的主要为肌醇物质，肌醇与火麻油中的磷脂能反应生成植酸；植酸具有很强的抗氧化性，提高火麻油的抗氧化作用，而且还可抑制具有强致癌作用的黄曲霉毒素的生成；同时植酸能促进机体脂肪代谢，降低血脂，抑制胆固醇的生成，提高了火麻油的保健价值。
利用生姜浸膏中含有的姜精油和姜辣素在高温下和火麻油发生美拉德反应，提高火麻油的香味，促进火麻油的风味；同时生姜蛋白酶能促进火麻油的出油率，提高初次提取滤渣中火麻油出油率。
110～170℃下，葡萄汁中的肌醇和火麻中的磷脂能最大化合成植酸，进一步提高火麻油中植酸的含量。
含碳的脂肪、蛋白质、胆固醇和糖等化合物在瞬间高温和低氧条件下发生了热裂解过程，再经过环合反应、聚合反应以及生焦等过程形成了大量以苯并(α)芘为主的稠环芳烃，苯并(α)芘具有致癌性、致畸性及致基因突变性；黄连根茎含有多种异喹啉生物碱，这类生物碱结构中含有碳杂环和季铵盐结构，对苯并(α)芘具有清除作用；黄连生物碱的活性物质部分保留于火麻油中，进一步提高了火麻油的营养价值。
作为本发明的进一步改进，步骤(2)所述粉碎后的火麻仁粉平均粒径为180～200目。
作为本发明的进一步改进，步骤(3)所述葡萄汁制备方法为：取新鲜无病害葡萄进行榨 汁，离心过滤后取上清液，加水稀释至10～20倍。
作为本发明的进一步改进，步骤(5)所述破乳率为93～94％。
作为本发明的进一步改进，步骤(6)所述生姜浸膏的制备方法如下：
取生姜洗净、去皮、凉干后，切成1～2mm的薄片，采用无水乙醇按照料液比1∶6于50℃恒温水浴中提取4h，过滤，滤液采用真空旋转蒸发浓缩至干，然后溶于100mL水中，加入等体积的乙酸乙酯，萃取3次，合并乙酸乙酯层，真空旋蒸浓缩得到生姜浸膏。
作为本发明的进一步改进，步骤(7)所述的负载黄连总生物碱吸附溶液中各物质含量分别为：巴马汀11～13mg/ml、小劈柴34～36mg/ml、黄连碱20.～22mg/ml。
作为本发明的进一步改进，步骤(7)所述的负载黄连总生物碱吸附溶液制备方法如下：
取活性炭纤维材料，加入黄连总生物碱溶液，在40℃水温下搅拌吸附90min，制备成负载黄连总生物碱80～120ml/g的吸附溶液。
活性炭纤维具有较大的比表面积和微孔容积，吸附量大，吸附速度快，因此负载黄连生物碱的活性炭纤维能快速的吸附火麻油中的苯并(α)芘；活性炭纤维不溶于油中，易于离心分离。
本发明的有益效果：
1、本发明制备工艺简单，原料获取简单，均为天然植物材料，成本低毒害物质低，同时各工艺反应条件易于控制；
2、本发明利用含有对人体具有保健价值的葡萄汁、姜和黄连辅助火麻油提取，不仅提高火麻油的提取率，增加了火麻油的香味，同时提高了火麻油的保健价值。
具体实施方式
下面结合实施例对本发明作进一步说明。
实施例1
(1)去除火麻仁的杂质，然后烘烤火麻仁使含水量降至7％，然后对烘干后的火麻仁进行脱皮；将脱皮后的火麻仁采用刀片式中药粉碎机进行粉碎，得到平均粒径为180目的火麻仁粉；
(2)将火麻仁粉与葡萄汁按料液比为1∶1混合均匀，调节pH为9，反应温度为70℃，浸提0.5h后得到反应液；
所述葡萄汁制备方法为：取新鲜无病害葡萄进行榨汁，离心过滤后取上清液，加水稀释至10倍；
(4)将反应液于3000r/min下离心分离20min，得到油相I、水相I、乳状液和沉淀；
(5)取乳状液于5℃下冷冻至凝结，然后将其置于35℃下放置破乳40min，8000r/min下离心15～20min，破乳率为93％，得到油相II和水相II；
(6)将水相I、水相II混合均匀，加热浓缩至原体积的10％，然后按料液比1∶6加入生姜浸膏混合均匀，于50℃下水水浴加热1.5h，得到水解液；
所述生姜浸膏的制备方法如下：取生姜洗净、去皮、凉干后，切成1～2mm的薄片，采用无水乙醇按照料液比1∶6(m/v)于50℃恒温水浴中提取4h，过滤，滤液采用真空旋转蒸发浓缩至干，然后溶于100mL水中，加入等体积的乙酸乙酯，萃取3次，合并乙酸乙酯层，真空旋蒸浓缩得到生姜浸膏；
(7)将油相I和油相II混合均匀得到混合油，然后加入步骤(6)所得水解液，再加入混合油体积5％的负载黄连总生物碱吸附溶液，混合均匀后转入高压反应釜中，加热升温到110℃后保温10～20min，然后冷却至室温，离心分离去除水相和杂质，即可得到火麻油；
所述的负载黄连总生物碱吸附溶液中各物质含量分别为：巴马汀11％、小劈柴34％、黄连碱20％；
制备方法如下：取活性炭纤维材料，加入黄连生物碱溶液，在40℃水温下搅拌吸附90min，制备成80mg/g的负载黄连总生物碱吸附溶液。
本实施例中，火麻油提取率为36.4％。
实施例2
(1)去除火麻仁的杂质，然后烘烤火麻仁使含水量降至12％，然后对烘干后的火麻仁进行脱皮；将脱皮后的火麻仁采用刀片式中药粉碎机进行粉碎，得到平均粒径为200目的火麻仁粉；
(2)将火麻仁粉与葡萄汁按料液比为1∶5混合均匀，调节pH为11，反应温度为80℃，浸提1.5h后得到反应液；
所述葡萄汁制备方法为：取新鲜无病害葡萄进行榨汁，离心过滤后取上清液，加水稀释至20倍；
(4)将反应液于3000r/min下离心分离50min，得到油相I、水相I、乳状液和沉淀；
(5)取乳状液于-1℃下冷冻至凝结，然后将其置于40℃下放置破乳40min，8000r/min下离心15～20min，破乳率为94％，得到油相II和水相II；
(6)将水相I、水相II混合均匀，加热浓缩至原体积的20％，然后按料液比1∶10加入生姜浸膏混合均匀，于60℃下水水浴加热2h，得到水解液；
所述生姜浸膏的制备方法如下：取生姜洗净、去皮、凉干后，切成1～2mm的薄片，采用 无水乙醇按照料液比1∶6(m/v)于50℃恒温水浴中提取4h，过滤，滤液采用真空旋转蒸发浓缩至干，然后溶于100mL水中，加入等体积的乙酸乙酯，萃取3次，合并乙酸乙酯层，真空旋蒸浓缩得到生姜浸膏；
(7)将油相I和油相II混合均匀得到混合油，然后加入步骤(6)所得水解液，再加入混合油体积10％的负载黄连总生物碱吸附溶液，混合均匀后转入高压反应釜中，加热升温到170℃后保温10～20min，然后冷却至室温，离心分离去除水相和杂质，即可得到火麻油；
所述的负载黄连总生物碱吸附溶液中各物质含量分别为：巴马汀13％、小劈柴36％、黄连碱22％；
制备方法如下：取活性炭纤维材料，加入黄连生物碱溶液，在40℃水温下搅拌吸附90min，制备成120mg/g的负载黄连总生物碱吸附溶液。
本实施例中，火麻油的提取率为36.9％。
实施例3
(1)去除火麻仁的杂质，然后烘烤火麻仁使含水量降至7～12％，然后对烘干后的火麻仁进行脱皮；将脱皮后的火麻仁采用刀片式中药粉碎机进行粉碎，得到平均粒径为180～200目的火麻仁粉；
(2)将火麻仁粉与葡萄汁按料液比为1∶3混合均匀，调节pH为10，反应温度为75℃，浸提1h后得到反应液；
所述葡萄汁制备方法为：取新鲜无病害葡萄进行榨汁，离心过滤后取上清液，加水稀释至12倍；
(4)将反应液于3000r/min下离心分离40min，得到油相I、水相I、乳状液和沉淀；
(5)取乳状液于1℃下冷冻至凝结，然后将其置于38℃下放置破乳35min，8000r/min下离心20min，破乳率为94％，得到油相II和水相II；
(6)将水相I、水相II混合均匀，加热浓缩至原体积的15％，然后按料液比1∶8加入生姜浸膏混合均匀，于55℃下水水浴加热2h，得到水解液；
所述生姜浸膏的制备方法如下：取生姜洗净、去皮、凉干后，切成1～2mm的薄片，采用无水乙醇按照料液比1∶6(m/v)于50℃恒温水浴中提取4h，过滤，滤液采用真空旋转蒸发浓缩至干，然后溶于100mL水中，加入等体积的乙酸乙酯，萃取3次，合并乙酸乙酯层，真空旋蒸浓缩得到生姜浸膏；
(7)将油相I和油相II混合均匀得到混合油，然后加入步骤(6)所得水解液，再加入混合油体积8％的负载黄连总生物碱吸附溶液，混合均匀后转入高压反应釜中，加热升温到 135℃后保温10～20min，然后冷却至室温，离心分离去除水相和杂质，即可得到火麻油；
所述的负载黄连总生物碱吸附溶液中各物质含量分别为：巴马汀12％、小劈柴35％、黄连碱21％；
制备方法如下：取活性炭纤维材料，加入黄连生物碱溶液，在40℃水温下搅拌吸附90min，制备成110mg/g的负载黄连总生物碱吸附溶液。
本实施例中火麻油提取率为37.2％。
对比实施例
本实施例为专利CN201210127891.8中的技术方案，具体如下：
超声波辅助超临界C02萃取火麻油的方法，其包括如下步骤：
(1)预处理将火麻仁中的杂质清除后，然后在50℃下烘至火麻仁中的含水量降至7％，进行机械粉碎，过筛分级，获得30目火麻仁粉；
(2)准确称取上述火麻仁粉50g并均匀拌入二氧化硅5g，混合均匀；
(3)将步骤(2)处理的火麻仁粉加入超临界提取设备中的提取罐中，并加装超声波发生装置，旋紧密封；设定萃取压力25MPa、萃取温度40℃；分离釜压力5MPa，温度35℃，设定CO2流量20L/h，萃取时间为6小时；超声波辅助提取条件为：超声频率为20KHz，超声功率密度100W/L。每隔30分钟从分离釜出料口收集萃取物。此工艺条件下火麻仁提油率为28.4％。
与本发明相比，对比实施例中的提油率低，同时设备要求高，成本高。
针对实施例1～3制得的火麻油和对比实施例制得的火麻油进行食用测试，随机选取50名实验者，男女各半，让他们分别食用实施例制得火麻油和对比实施例制得的火麻油10天，然后对两种火麻油的各项感官口味进行打分，满分5份，分越高表示感官口味越好，计算平均分汇总成表1。
表1 火麻油食用实验结果
Figure PCTCN2018000041-appb-000001
由表1可以看出，相比对比实施例的火麻油，参与实验的人们本发明实施例制备得的火麻油有更好的口碑，由此可知本发明制备的火麻油具有很好的价值。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明 的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。

Claims (7)

  1. 一种火麻油的提取工艺，其特征在于：包括以下步骤：
    (1)去除火麻仁的杂质，然后烘烤火麻仁使含水量降至7～12％，然后对烘干后的火麻仁进行脱皮；将脱皮后的火麻仁采用刀片式中药粉碎机进行粉碎，得到火麻仁粉；
    (2)将火麻仁粉与葡萄汁按料液比为1∶(1～5)混合均匀，调节pH为9～11，反应温度为70～80℃，浸提0.5～1.5h后得到反应液；
    (4)将反应液于3000r/min下离心分离20～50min，得到油相I、水相I、乳状液和沉淀；
    (5)取乳状液于-1～5℃下冷冻至凝结，然后将其置于35～40℃下放置破乳30～40min，8000r/min下离心15～20min，得到油相II和水相II；
    (6)将水相I、水相II混合均匀，加热浓缩至原体积的10～20％，然后按料液比1∶(6～10)加入生姜浸膏混合均匀，于50～60℃下水水浴加热1.5～2h，得到水解液；
    (7)将油相I和油相II混合均匀得到混合油，然后加入步骤(6)所得水解液，再加入混合油体积5～10％的负载黄连总生物碱吸附溶液，混合均匀后转入高压反应釜中，加热升温到110～170℃后保温10～20min，然后冷却至室温，离心分离去除水相和杂质，即可得到火麻油。
  2. 根据权利要求1所述的火麻油的提取工艺，其特征在于：步骤(2)所述粉碎后的火麻仁粉平均粒径为180～200目。
  3. 根据权利要求1所述的火麻油的提取工艺，其特征在于：步骤(3)所述葡萄汁制备方法为：取新鲜无病害葡萄进行榨汁，离心过滤后取上清液，加水稀释至10～20倍。
  4. 根据权利要求1所述的火麻油的提取工艺，其特征在于：步骤(5)所述破乳率为93～94％。
  5. 根据权利要求1所述的火麻油的提取工艺，其特征在于：步骤(6)所述生姜浸膏的制备方法如下：取生姜洗净、去皮、凉干后，切成1～2mm的薄片，采用无水乙醇按照料液比1∶6于50℃恒温水浴中提取4h，过滤，滤液采用真空旋转蒸发浓缩至干，然后溶于100ml水中，加入等体积的乙酸乙酯，萃取3次，合并乙酸乙酯层，真空旋蒸浓缩得到生姜浸膏。
  6. 根据权利要求1所述的火麻油的提取工艺，其特征在于，步骤(7)所述的负载黄连总生物碱吸附溶液中，各物质含量分别为：巴马汀11～13mg/ml、小劈柴34～36mg/ml、黄连碱20～22mg/ml。
  7. 根据权利要求1所述的火麻油的提取工艺，其特征在于：步骤(7)所述的负载黄连总生物碱吸附溶液制备方法如下：取活性炭纤维材料，加入黄连总生物碱溶液，在40℃水温下搅拌吸附90min，制备成负载黄连总生物碱80～120ml/g的吸附溶液。
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