CN107501286B - 一种芝麻木脂素提取物的制备方法 - Google Patents
一种芝麻木脂素提取物的制备方法 Download PDFInfo
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- CN107501286B CN107501286B CN201710721693.7A CN201710721693A CN107501286B CN 107501286 B CN107501286 B CN 107501286B CN 201710721693 A CN201710721693 A CN 201710721693A CN 107501286 B CN107501286 B CN 107501286B
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- Prior art keywords
- sesame
- extract
- extraction
- mixture
- sesame lignans
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- 235000007221 pinoresinol Nutrition 0.000 description 8
- BURBOJZOZGMMQF-UHFFFAOYSA-N xanthoxylol Natural products C1=C(O)C(OC)=CC=C1C1C(COC2C=3C=C4OCOC4=CC=3)C2CO1 BURBOJZOZGMMQF-UHFFFAOYSA-N 0.000 description 8
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- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/357—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having two or more oxygen atoms in the same ring, e.g. crown ethers, guanadrel
- A61K31/36—Compounds containing methylenedioxyphenyl groups, e.g. sesamin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/44—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D317/46—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 ortho- or peri-condensed with carbocyclic rings or ring systems condensed with one six-membered ring
- C07D317/48—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring
- C07D317/62—Methylenedioxybenzenes or hydrogenated methylenedioxybenzenes, unsubstituted on the hetero ring with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to atoms of the carbocyclic ring
- C07D317/64—Oxygen atoms
-
- 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
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0021—Preserving by using additives, e.g. anti-oxidants containing oxygen
-
- 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
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0085—Substances of natural origin of unknown constitution, f.i. plant extracts
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Botany (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- General Health & Medical Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mycology (AREA)
- Medicinal Chemistry (AREA)
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Abstract
本发明公开了一种芝麻木脂素提取物的制备方法：取冷榨白芝麻饼粕烘干，粉碎成粉末，浸没于酸化乙醇溶液中，将混合物置于超声‑微波协同萃取器中提取，离心得上清液，将所得上清液旋转蒸发得芝麻木脂素提取物粗品；所述的酸化乙醇溶液为氯化氢标准溶液和无水乙醇的混合物；所述的混合物中，氯化氢的质量分数为1～3％，无水乙醇的质量分数为88.9～96.7％，余量为水；将所得芝麻木脂素提取物粗品在室温下用正己烷萃取，合并萃取液，将所得萃取液旋转蒸发浓缩至浸膏状干燥得到芝麻木脂素提取物。本发明制备过程无有毒有害有机溶剂；所得产物无需精细纯化，成本较低；可以防止或抑制氧化酸败，增加食用油的多种保健功能。
Description
(一)技术领域
本发明涉及食用油脂加工贮藏领域,具体涉及一种芝麻木脂素提取物的制备方法。
(二)背景技术
芝麻的主要成分是油脂，含量约为50％，其次是蛋白质，约占20％，另外还含有各种维生素、碳水化合物、矿物质、食物纤维以及作为芝麻特征成分的木脂素类化合物。芝麻木脂素(sesame lignans)是芝麻的特征活性成分，主要包括脂溶性木脂素(lignans)和含有配糖体的水溶性木脂素(lignan glucosides)。脂溶性木脂素有芝麻素(sesamin)、芝麻林素(sesamolin)、芝麻素酚(sesaminol)和芝麻酚(sesamol)等，其结构如下所示；
水溶性木脂素则是由以上木脂素和1～3个葡萄糖相连形成的极性较强的糖苷。芝麻原料中木脂素质量分数为0.5％～1％，芝麻林素在芝麻木脂素中的含量居于第2位，约占芝麻的0.1％～0.3％，仅次于质量分数为0.2％～0.5％的芝麻素，其余几种含量极微。芝麻木脂素在生物体内具有稳定血压、降血糖、降血脂，保护肝脏、抗菌防腐和抗癌抑瘤等多种生物活性，具有重要的营养价值和药理作用，更为可贵的是它是一类天然绿色的抗氧化剂，符合人们对安全无毒高效的迫切要求。
我国芝麻资源丰富，目前主要应用于芝麻油的生产，制油过程中的副产品芝麻渣或芝麻饼粕作为废物被丢弃或者是用作为饲料和肥料，造成资源极大浪费，芝麻原料制油后的副产物芝麻饼粕年产量达50万吨以上，研究表明其中依然含有一定量的芝麻木脂素类化合物。近二十年来，有关芝麻木脂素的生理功能的研究取得较大进展，显示它具有抑制△5不饱和酶、降低胆固醇、抗高血压、抗菌、保护肝脏、抑制乳癌、免疫激活和抗氧化等生理作用。
植物油脂受温度、光照、氧、金属离子及微生物等作用，会发生自氧化，其自氧化是一个典型的自由基连锁氧化反应，首先是油脂在单重态氧的引发下生成脂肪自由基(R·)，进一步氧化，生成过氧自由基(ROO·)，后者再夺取未被氧化的不饱和脂肪酸的氢，而形成氢过氧化物和新的脂肪自由基(R·)，通过链式反应依次传递，直至产生稳定的化合物，导致食品酸败。长期摄入这种酸败食品会导致细胞功能减退乃至组织坏死，诱发癌症、心血管病等。防止油脂氧化酸败的方法很多，世界各国广泛使用的是添加人工合成抗氧化剂，如BHT、BHA、TBHQ等有较多的副作用，因此许多国家对它们的使用进行了限制，有的国家已经禁止使用。随着经济与社会的发展，以及人们对食品质量安全要求的提高，开发营养多功能、安全可靠的天然抗氧化剂成为当前的研究热点。
芝麻油与其他植物油相比，因为含有芝麻素、芝麻酚、芝麻林素等内源性木脂素类抗氧化剂，使芝麻尽管含有高含量不饱和酸而仍有较好的储藏稳定性。近些年研究发现，含有游离酚羟基的芝麻酚和芝麻素酚，相对芝麻素具有更突出的抗氧化能力和体内活性。在酸性条件下，芝麻林素易发生分解反应和傅克－烷基化反应，生成芝麻酚和芝麻素酚。但是已有的文献中采用纯品，价格较高，而且该反应一般需要催化剂，如磷钨酸，还需石油醚、丙酮、甲苯等有毒有机溶剂介质存在条件下进行反应{李雪芳等.反应介质对芝麻林素转化生成芝麻素酚的影响[J].中国粮油学报，2015,30(3):111-115}，在食品中的应用安全性较差。芝麻素在酸性条件下容易水解，转化为松脂酚(Pinoresinol)，松脂酚也具有比芝麻素更强的抗氧化性。
目前有关芝麻及其饼粕木脂素提取、抗氧化、芝麻素类化合物反应转化及食用油添加的文献已有不少。陕西源邦生物的赵江等人“一种从芝麻粕中制备高含量芝麻素的方法”(申请公布号CN 104177370A)，发明涉及一种从芝麻粕中制备高含量芝麻素的方法，渗流、浓缩、树脂除色素、纯化、浓缩、结晶等步骤。军事医学科学的陈伟强等人“一种从芝麻饼粕中得到高纯度芝麻素的制备工艺”，(申请公布号CN 101735234 A)，发明提供了一种从芝麻饼粕中得到高纯度芝麻素的制备工艺，将芝麻饼粕通过正己烷等有机溶剂在特定条件下进行一系列提取纯化，最终得到高纯度的芝麻素。安徽省阜阳的刘勇等人“一种利用芝麻饼粕提取芝麻素的方法”，以芝麻油厂废弃物饼粕为原料，从芝麻饼粕中提取芝麻素。南京泽朗医药的刘东锋等人“一种从芝麻中制备芝麻素的方法”(申请公布号CN 101817827 A)，发明以芝麻为原料，食用乙醇回流提取，大孔树脂纯化、结晶等步骤。江苏大学的董英等人“一种从芝麻饼粕中提取芝麻素的制备方法”(公开号CN 101007827A)，发明涉及一种从芝麻饼中制备芝麻素的方法，其以芝麻油厂的副产品芝麻饼粕为原料，先用正己烷脱除剩余的油脂，以此脱脂的芝麻饼为原料，用甲醇提取芝麻素粗提物，再用硅胶柱层析法对粗提物进行分离纯化，得到的芝麻素产品得率为1.57％，纯度为88.02％。日本三得利的“高含量表芝麻素的组合物的制造方法及装置”(公开号CN 1939921 A)，发明是简便且高收率地制造基于芝麻素和表芝麻素的合计重量，含有浓度大于50％重量的表芝麻素的组合物的方法及装置。以上文献和专利中大多采用溶剂直接加热提取芝麻或饼粕中的芝麻木脂素，有些经过了后续分离纯化，部分采用人工化学合成的芝麻酚等，对食用油进行添加抗氧化研究和应用。从效果来看，添加的芝麻木脂素油脂氧化稳定性普遍不如BHT、BHA、TBHQ等人工合成的抗氧化剂；从芝麻原料直接提取芝麻素成本较高，分离纯化则步骤繁琐，操作复杂，难以产业化，同时在抗氧化时还存在多种成分的协同作用，单一纯品往往不如几种混合物；现有的人工合成芝麻酚等木脂素成分，及芝麻林素纯品化学反应转化芝麻酚和芝麻素酚，在传统化学反应中不可避免使用有毒有害催化剂及有机溶剂，在食品抗氧化的食用安全性上存在较大问题，另外现有文献普遍以黑芝麻为原料，所得提取物如果未经后续分离纯化，所得产物颜色较深，影响后续的食用油添加的色泽。
(三)发明内容
为解决现有技术存在的问题，本发明的目的在于提供一种芝麻木脂素提取物的制备方法，以白芝麻饼粕为原料，采用酸性乙醇为介质，超声-微波耦合法萃取转化，无有毒有害化学成分残留，获得含较高芝麻酚、芝麻木素酚等成分的芝麻木脂素提取物。
一种芝麻木脂素提取物的制备方法，所述方法具体按如下步骤进行：
(1)取冷榨白芝麻饼粕烘干，粉碎成粉末，浸没于酸化乙醇溶液中，将混合物置于超声-微波协同萃取器中提取，离心得上清液，将所得上清液旋转蒸发得芝麻木脂素提取物粗品；所述的酸化乙醇溶液为氯化氢标准溶液和无水乙醇的混合物；所述的混合物中，氯化氢的质量分数为1～3％，无水乙醇的质量分数为88.9～96.7％，余量为水；
(2)将步骤(1)所得芝麻木脂素提取物粗品在室温下用正己烷萃取，合并萃取液，将所得萃取液旋转蒸发浓缩至浸膏状干燥得到芝麻木脂素提取物。
进一步，推荐本发明所述方法按具体如下步骤进行：
(1)取冷榨白芝麻饼粕于50～60℃下烘干，粉碎过60～80目筛得粉末，浸没于酸化乙醇溶液中，将混合物置于超声-微波协同萃取器中在50～70℃下提取10～30min，离心得上清液，将所得上清液在40～50℃旋转蒸发得芝麻木脂素提取物粗品；所述的酸化乙醇溶液为氯化氢标准溶液和无水乙醇的混合物；所述的混合物中，氯化氢的质量分数为1～3％，无水乙醇的质量分数为88.9～96.7％，余量为水；
(2)将步骤(1)所得芝麻木脂素提取物粗品在室温下用正己烷萃取2～3次，合并萃取液，将所得萃取液在40～50℃下旋转蒸发浓缩至浸膏状干燥得到芝麻木脂素提取物。
进一步，步骤(1)中，所述的冷榨白芝麻饼粕为新鲜白芝麻饼粕在70～90℃下二次冷榨得到，然后塑料袋密封后-18℃冷冻备用。
进一步，步骤(1)中，所述的酸化乙醇的水溶液的加入量以所述的冷榨白芝麻饼粕的质量计为10～20ml/g。
进一步，步骤(1)中，所述的超声频率定频25KHz，功率为300～600W。
进一步，步骤(1)中，所述的微波频率定频2450MHz，功率为300～600W。
再进一步，步骤(2)中，所述的正己烷的加入量以所述的芝麻木脂素提取粗品的质量计为50～100ml/g。
测定通过上述制备方法制得的芝麻木脂素提取物在食用油抗氧化方面的性能。
将所得芝麻木脂素提取物称重并进行木脂素成分及含量HPLC分析，然后向新鲜压榨食用菜籽油添加0.01％～0.1％的木脂素提取物，充分搅拌震荡混匀，并进行贮藏氧化稳定性(POV)测定，过氧化值(POV)测定：采用GB 5009.227-2016，分析结果以1kg样品中活性氧的毫摩尔数表示过氧化值(mmol/kg)。
与现有技术相比，本发明的有益效果在于：
本发明以冷榨白芝麻饼粕为原料，可以有效减少资源浪费，降低废物排放，实现农产品资源的进一步有效利用，经酸化乙醇溶液超声-微波协同萃取/合成仪，提取过程同时耦合目标产物转化(芝麻林素转化为抗氧化更强的芝麻酚和芝麻素酚，芝麻素转化为松脂酚，芝麻木脂素苷水解成脂溶性的芝麻木脂素)，制备过程无有毒有害有机溶剂；所得产物无需精细纯化，成本较低；颜色为浅黄色，不影响食用油添加后的色泽；同等浓度下对食用油的抗氧化效果接近或优于现有的BHT；不仅可以防止或抑制氧化酸败，还可以增加食用油的多种保健功能。
(四)附图说明
图1为芝麻木脂素标准品HPLC谱图；
图2为微波超声耦合样品HPLC谱图；
图3为常规乙醇回流提取样品HPLC谱图；
图4为菜籽油添加后的氧化稳定性；
图5为菜籽油添加案例1的芝麻饼粕木脂素后氧化稳定性；
图6为菜籽油添加案例2的芝麻饼粕木脂素后氧化稳定性；
图7为制备工艺流程图。
(五)具体实施方式
本发明所述的超声-微波协同萃取器为电脑微波超声波组合催化合成/萃取仪，BILON-CW-1000，上海比朗仪器制造有限公司，配BILON-W-501S型低温冷却液循环装置。
所述的旋转蒸发器型号为R2002B，配循环水泵，上海申生科技有限公司。
木脂素成分及含量测定：通过HPLC检测，具体条件如下：WATERS1525高效液相色谱仪，色谱柱：Cosmosil C18(4.6mm*250mm，填充粒度5μm)；WATERS 2487紫外检测器；流动相：甲醇(A)-水(B)(梯度洗脱)，检测波长287nm，条件见表1，流速1.0mL/min，进样量20μL，以芝麻酚、芝麻素酚、芝麻素和芝麻林素标准品(购自sigma公司)为对照，进行定性(保留时间)和定量(峰面积归一化)分析，标准品HPLC见图1，耦合萃取和常规乙醇萃取样品HPLC分析分别见图2和图3，其中松脂酚也采用标准品对照。
表1流动相梯度洗脱条件
贮藏稳定性(POV)测定
准确称取油样适量，分别加入油样质量的0.01％～0.1％的木脂素提取物、空白对照、BHT对照，干净玻璃棒搅拌后，继续用旋涡震荡器震荡5min至混合均匀，采用Schaal烘箱法加速测定油脂氧化稳定性敞口放入(63±1)℃的恒温烘箱中进行强制氧化，每隔24h搅拌1次，并交换1次位置，取样测定POV值，每组实验重复3次，取平均值，连续测定7天。
实施例1：
称取冷榨芝麻饼粕50g→60℃烘干→70目粉碎过筛→加入800mL的酸化乙醇溶液(氯化氢质量分数2％，水质量分数5.4％，乙醇质量分数92.6％)超声微波萃取器提取，微波功率500W，超声功率500W，萃取温度60℃，萃取时间20min→5000r/min离心，50℃旋转蒸发得到芝麻木脂素提取物粗品2.36g→200mL正己烷萃取2次后合并萃取液→45℃，旋转蒸发浓缩干燥→称重得芝麻木脂素提取物0.67g(即提取率为1.34％)，经HPLC分析，其中含芝麻酚12.4mg(即含量为1.85％)、松脂酚10.5mg(1.57％)、芝麻素酚25.7mg(即含量为3.84％)、芝麻素86.3mg(即含量为12.88％)、芝麻林素16.2mg(即含量为2.42％)，上述总木脂素151.1mg(即含量为22.55％)→新鲜压榨食用菜籽油添加0.01％的木脂素提取物→充分搅拌震荡混匀→菜籽油灌装→取上述样品(并设空白和添加0.01％BHT菜籽油样品对照)，进行油脂氧化稳定性测定。
常规对照处理：称取冷榨芝麻饼粕50g→60℃烘干→70目粉碎过筛→加入1000mL无水乙醇沸腾回流提取；提取时间30min→5000r/min离心得上清液，40℃旋转蒸发至干，得到芝麻木脂素提取物粗品2.54g→250mL正己烷萃取2次后合并萃取液→40℃旋转蒸发浓缩干燥→芝麻木脂素提取物→称重得浅黄色芝麻木脂素提取物0.53g(即提取率为1.06％)，经HPLC分析，其中含芝麻酚12.4mg(即含量为1.85％)、芝麻素86.3mg(即含量为12.88％)、芝麻林素16.2mg(即含量为2.42％)，上述总木脂素151.1mg(即含量为22.55％)，未检测到芝麻酚、松脂酚和芝麻素酚→新鲜压榨食用菜籽油添加0.01％的木脂素提取物→充分搅拌震荡混匀→菜籽油PET瓶灌装→贮藏氧化稳定性(POV)测定
采用上述技术解决方案中的Schaal烘箱法测定油脂氧化稳定性，连续测定7天，结果见图4。
从图4可知，添加0.01％的耦合萃取的芝麻饼粕木脂素的菜籽油，其贮藏效果略优于同等浓度的阳性对照BHT，而添加0.01％的常规乙醇提取木脂素其贮藏效果则略逊于同等浓度的阳性对照BHT，三者都显著远优于空白对照组，耦合提取有组于抗氧化成分的萃取和转化。(63±1)℃烘箱贮藏21d后，耦合提取芝麻木脂素POV值为4.8mmol/kg，仍小于GB1536-2004菜籽油的一级、二级压榨菜籽油5.0mmol/kg的限定标准；而BHT的相应值为5.9mmol/kg，介于一级、二级压榨菜籽油5.0mmol/kg和三级、四级压榨菜籽油6.0mmol/kg限定标准。
实施例2
称取冷榨白芝麻饼粕50g→50℃烘干→60目粉碎过筛→加入500mL的酸化乙醇溶液(氯化氢质量分数1％，水质量分数2.7％，乙醇质量分数96.3％)超声微波萃取器提取，微波功率300W，超声功率300W；萃取温度50℃，萃取时间10min→5000r/min离心得上清液，45℃旋转蒸发至干，得到芝麻木脂素提取物粗品1.92g→150mL正己烷萃取2次后合并萃取液→45℃旋转蒸发浓缩干燥→芝麻木脂素提取物→称重得浅黄色提取物0.51g(即提取率为1.03％)，经HPLC分析，其中含芝麻酚6.3mg(即含量为1.23％)、松脂酚7.7mg(1.51％)、芝麻素酚18.5mg(即含量为3.63％)、芝麻素57.9mg(即含量为11.35％)、芝麻林素13.8mg(即含量为2.71％)，上述总木脂素104.2mg(即含量为20.43％)其中含芝麻酚16mg(即含量为3.1％)、芝麻素57mg(即含量为12.5％)、芝麻林素32mg(即含量为6.3％)，总木脂素105mg(即含量为20.6％)→新鲜压榨食用菜籽油分别添加0.01％和0.02％的木脂素提取物→充分搅拌震荡混匀→菜籽油PET瓶灌装→贮藏氧化稳定性(POV)测定(结果见图5)
从图5可知，添加实施例2的0.01％芝麻饼粕木脂素的菜籽油，其贮藏效果略次于同等浓度的阳性对照BHT，但远优于空白对照组。而添加实施例2的0.02％芝麻饼粕木脂素的菜籽油，其贮藏效果略优于0.01％的BHT，(63±1)℃烘箱贮藏21d后，其POV值为4.6mmol/kg，小于GB1536-2004菜籽油的一级、二级压榨菜籽油5.0mmol/kg的限定标准。
实施例3
称取冷榨白芝麻饼粕50g→55℃烘干→80目粉碎过筛→加入1000mL的酸化乙醇溶液(氯化氢质量分数3％，水质量分数8.1％，乙醇质量分数88.9％)超声微波萃取器提取，微波功率600W；超声功率600W；萃取温度70℃，萃取时间30min→5000r/min离心得上清液，45℃旋转蒸发至干，得到芝麻木脂素提取物粗品2.79g→170mL正己烷萃取3次后合并萃取液→45℃旋转蒸发浓缩干燥→芝麻木脂素提取物→称重得浅黄色芝麻木脂素提取物0.79g(即提取率为1.58％)，经HPLC分析，其中含芝麻酚15.5mg(即含量为1.96％)、松脂酚14.9mg(1.89％)、芝麻素酚33.6mg(即含量为4.25％)、芝麻素116.8mg(即含量为14.78％)、芝麻林素22.6mg(即含量为2.86％)，上述总木脂素203.4mg(即含量为25.75％)→新鲜压榨食用菜籽油分别添加0.01％和0.02％的木脂素提取物→充分搅拌震荡混匀→菜籽油PET瓶灌装→贮藏氧化稳定性(POV)测定(结果见图6)。
从图6可知，仅添加实施例3的0.01％芝麻饼粕木脂素的菜籽油，其贮藏效果就略优于添加0.02％的阳性对照BHT，且远优于空白对照组。添加实施例3的0.01％芝麻饼粕木脂素的菜籽油，(63±1)℃烘箱贮藏21d后，其POV值为4.2mmol/kg，小于GB1536-2004菜籽油的一级、二级压榨菜籽油5.0mmol/kg的限定标准；而添加0.02％BHT的相应值为4.7mmol/kg。
Claims (7)
1.一种芝麻木脂素提取物的制备方法，其特征在于：所述方法具体按如下步骤进行：
(1)取冷榨白芝麻饼粕烘干，粉碎成粉末，浸没于酸化乙醇溶液中，将混合物置于超声-微波协同萃取器中提取，离心得上清液，将所得上清液旋转蒸发得芝麻木脂素提取物粗品；所述的酸化乙醇溶液为氯化氢标准溶液和无水乙醇的混合物；所述的混合物中，氯化氢的质量分数为1～3％，无水乙醇的质量分数为88.9～96.7％，余量为水；
(2)将步骤(1)所得芝麻木脂素提取物粗品在室温下用正己烷萃取，合并萃取液，将所得萃取液旋转蒸发浓缩至浸膏状干燥得到芝麻木脂素提取物。
2.如权利要求1所述的制备方法，其特征在于：所述方法具体按如下步骤进行：
(1)取冷榨白芝麻饼粕于50～60℃下烘干，粉碎过60～80目筛得粉末，浸没于酸化乙醇溶液中，将混合物置于超声-微波协同萃取器中在50～70℃下提取10～30min，离心得上清液，将所得上清液在40～50℃旋转蒸发得芝麻木脂素提取物粗品；所述的酸化乙醇溶液为氯化氢标准溶液和无水乙醇的混合物；所述的混合物中，氯化氢的质量分数为1～3％，无水乙醇的质量分数为88.9～96.7％，余量为水；
(2)将步骤(1)所得芝麻木脂素提取物粗品在室温下用正己烷萃取2～3次，合并萃取液，将所得萃取液在40～50℃下旋转蒸发浓缩至浸膏状干燥得到芝麻木脂素提取物。
3.如权利要求1或2所述的方法，其特征在于：步骤(1)中，所述的冷榨白芝麻饼粕为新鲜白芝麻饼粕在70～90℃下二次冷榨得到。
4.如权利要求1或2所述的方法，其特征在于：步骤(1)中，所述的酸化乙醇溶液的加入量以所述的冷榨白芝麻饼粕的质量计为10～20ml/g。
5.如权利要求2所述的方法，其特征在于：步骤(1)中，所述的超声频率定频25KHz，功率为300～600W。
6.如权利要求2所述的方法，其特征在于：步骤(1)中，所述的微波频率定频2450MHz，功率为300～600W。
7.如权利要求2所述的方法，其特征在于：步骤(2)中，所述的正己烷的加入量以所述的芝麻木脂素提取物粗品的质量计为50～100ml/g。
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