CN112516113A - 一种杏鲍菇三萜类化合物纳米微胶囊制备方法 - Google Patents
一种杏鲍菇三萜类化合物纳米微胶囊制备方法 Download PDFInfo
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Abstract
本发明涉及一种杏鲍菇三萜类化合物纳米微胶囊制备方法，属于农产品精深加工领域。本发明将明胶、海藻酸钠作为壁材，明胶与海藻酸钠比例为1∶1，壁材总浓度为1％‑3％，将超声波辅助浸提得到的杏鲍菇三萜类化合物作为芯材，按照芯壁比1∶1混合，采用超声波分散2‑4min，再在10000‑13000PSI压力下高压微射流均质2‑4次，然后调节均质溶液温度15‑50℃，调节pH值3.6‑6.0，再加入0.1‑0.3％转谷氨酰胺酶固化，然后用去离子水和无水乙醇清洗，经过‑80℃～‑65℃超低温预冻6‑8h，最后在冷阱温度‑40℃～‑30℃，真空度25‑35pa，真空冷冻干燥46‑52h获得杏鲍菇三萜类化合物纳米微胶囊。本发明方法制备的杏鲍菇三萜类化合物纳米微胶囊包埋率达到75％以上，载药量达42％以上，微胶囊结构比较完好，构成的微胶囊外表形状呈球形，粒径基本均一，囊壁无破碎现象。
Description
技术领域
本发明涉及一种杏鲍菇三萜类化合物纳米微胶囊制备方法，属于农产品精深加工领域。
背景技术
杏鲍菇(Pleurotus eryngii)，又名刺芹侧耳，隶属于真菌门、担子菌纲、伞菌目、侧耳科、侧耳属。杏鲍菇菌肉肥厚，质地脆嫩，菌柄组织致密可全部食用，且菌柄比菌盖更脆滑、爽口，具有愉快的杏仁香味和鲍鱼口感，被称为“平菇王”。研究显示，杏鲍菇不仅富含蛋白质、碳水化合物、矿物质、维生素等营养物质，亦含有多种活性多糖、抗菌多肽、三萜和甾醇类等生物活性成分，具有极高的开发研究价值。特别是杏鲍菇中的三萜类化合物由于具有很强烈的“靶向杀灭”特性而引起科学工作者的兴趣。三萜类化合物(Triterpenoids)从结构上来说，是几个异戊二烯通过去掉羟基以后首尾相连接构成的物质，大多数的是30个碳原子，少数的含有27个碳原子的萜类化合物。三萜类化合物存在的形式、结构和性质根据在大自然中的植物体或者生物体中的不同，可以被分为三萜皂苷及苷元和其他三萜类化合物(包括苦味素、树脂、三萜醇和三萜生物碱等)两大类别。据研究报道，三萜类化合物具有良好的生物活性，化学反应活泼，结构独特，在保护肾脏和肝脏、抗菌、抗炎等方面很有价值，而且对于多种肿瘤如中枢神经系统和直肠癌、肺癌、乳腺癌等也有一定的抑制作用。
微胶囊技术是指将固体颗粒、液体微滴或气体作为胶囊的芯料，在其外部形成一层连续而极薄包裹的过程。微胶囊具有保护芯材物质免受环境影响，屏蔽味道、颜色、气味，改变物质重量、体积、状态或表面性能，隔离活性成分，降低挥发性和毒性，控制芯材物质的可持续释放等多种作用，目前该技术已经成为材料、化学、化工、生物和医学等诸多学科领域工作者的研究热点。纳米微胶囊，即具有纳米尺寸的微胶囊，粒径在1～1000nm之间，这是区别于一般微胶囊(粒径介于5～2000μm之间)的最重要的指标之一，其颗粒微小，易于分散和悬浮在水中，形成均一稳定的胶体溶液，并且具有良好的靶向性和缓释作用。
近年来，国内外关于杏鲍菇三萜类化合物的研究大多集中在提取纯化和功能活性分析，如中国专利CN201010158330.5公开了一种从杏鲍菇废菌渣中提取三萜类化合物的方法，天津大学李嗣乾等发表了关于超声波提取杏鲍菇三萜类化合物工艺的研究论文，天津大学李娇妹等发表了关于杏鲍菇三萜类化合物提取纯化工艺及抑制肿瘤活性研究论文，武汉设计工程学院凡芸等发表了关于超声辅助乙醇提取杏鲍菇总三萜化合物工艺研究论文。目前，尚未有关于杏鲍菇三萜类化合物纳米微胶囊制备方法的相关报道。
发明内容
技术问题
本发明的目的是提供一种杏鲍菇三萜类化合物纳米微胶囊制备方法。以杏鲍菇为原料提取其中的三萜类化合物，得到三萜类化合物的甲醇提取物，再以明胶、海藻酸钠为微胶囊的壁材，三萜类化合物为芯材，采用复合凝聚法进行包埋。由于明胶溶解于冰醋酸后分子链上产生大量带正电荷的氨基，海藻酸钠溶于水后的分子链上有大量带负电荷的羧基和羟基，在静电力作用下，可以通过正、负电荷吸引形成聚电解质膜，进而在高压微射流作用下对经过超声分散的三萜类化合物进行包裹，形成具有密封囊膜的微小粒子，起到保护芯材、隔离不相容组分、控制释放等功能。
技术方案
本发明所提供一种杏鲍菇三萜类化合物纳米微胶囊制备方法，包括以下步骤：
1.超声波辅助提取：称取300-500g经干燥并粉碎至80目的杏鲍菇粉末(含水率低于5％)，依照料液比1∶10加入甲醇，在室温下用磁力搅拌器搅拌浸提7-9h，然后用超声波浸提(超声功率100w，超声时间30min，间歇时间15s)，反复3-4次后归并提取液，待提取液冷却后减压过滤，再使用旋转蒸发器把滤液浓缩成浸膏，得到甲醇提取物，然后加入无菌水，用乙酸乙酯萃取3次，再用旋转蒸发器浓缩回收溶剂，得到乙酸乙酯提取物。
2.混合、分散、均质：在两个烧杯中分别称取1-3g明胶和海藻酸钠，倒入50-300ml蒸馏水搅拌，在50℃磁力搅拌器上搅拌1h使其充分溶解。在另外一个烧杯中混匀这两种溶液，然后按照1∶1芯壁比加入提取物。利用超声波分散溶液2-4min，获得分散平均的乳状液。最后采用高压微射流均质机在压力10000-13000PSI下对分散溶液均质2-4次。
3.调节温度和pH值：将经过均质的溶液倒入锥形瓶中，加入10％的冰醋酸溶液调节体系的pH值至(3.6)，在50℃水浴中搅拌1.5h，搅拌结束后，采取冰水浴的方法，将体系的温度降到15℃左右，然后用10％的氢氧化钠溶液将体系的pH值调到6.0。
4.固化、清洗：加入0.1％-0.3％的转谷氨酰胺酶，在磁力搅拌器上用低转速搅拌10-12h，获得固化的微胶囊分散液，然后将制得的微胶囊分散液静置分层、去上清液，减压过滤，用去离子水水洗得到湿囊，再用无水乙醇洗去湿囊表面未被包埋的三萜类化合物，最后将提取物倒入培养皿中，用保鲜膜封好。
5.冻干：将上述保鲜膜封好的培养皿放置在-80～-65℃超低温冰箱下预冻6-8h，再放到真空冷冻干燥腔体内，设置冷阱温度-40℃～-30℃，真空度25-35pa，真空冷冻干燥时间46-52h，最后得到粉末状纳米微胶囊。
有益效果
1.本发明方法制备的杏鲍菇三萜类化合物纳米微胶囊包埋率和载药量高。
2.本发明方法制备的杏鲍菇三萜类化合物纳米微胶囊结构比较完好，构成的微胶囊外表形状呈球形，囊壁无破碎现象。
3.本发明方法制备的杏鲍菇三萜类化合物纳米微胶囊粒径小且均一。
附图说明
图1杏鲍菇三萜类化合物纳米微胶囊粒径分布图
具体实施方式
下面的实施例可以更好地理解本发明，但不以任何方式限制本发明。
实施例
1.超声波辅助提取：称取380g经干燥并粉碎至80目的杏鲍菇粉末(含水率低于5％)，依照料液比1∶10加入甲醇(3800ml)，在室温下用PC-420D型磁力搅拌器(美国康宁公司)搅拌浸提7-9h，然后采用KH7200DB型超声波清洗机(昆山禾创超声仪器有限公司)超声处理30min，设置超声功率100w，间歇时间为15s，反复3次后归并提取液，待提取液冷却后减压过滤，再使用RE-52A型旋转蒸发器(上海亚荣生化仪器厂)把滤液浓缩成浸膏，得到甲醇提取物，然后加入无菌水中，用乙酸乙酯萃取3次，再用RE-52A型旋转蒸发器(上海亚荣生化仪器厂)浓缩回收溶剂，得到乙酸乙酯提取物。
2.混合、分散、均质：在两个烧杯中分别称取1g明胶和海藻酸钠，倒入100ml蒸馏水搅拌，在PC-420D型磁力搅拌器(美国康宁公司)50℃温度下搅拌1h使其溶解充分。在另外一个烧杯中混匀这两种溶液，然后按照1∶1芯壁比加入提取物。采用KH7200DB超声波清洗机(昆山禾创超声仪器有限公司)使溶液超声分散3min，获得分散平均的乳状液，再采用LM20高压微射流均质机(美国Microfluidics公司)在压力12000PSI下均质3次。
3.调节温度和pH值：将经过均质的溶液倒入锥形瓶中，加入10％的冰醋酸溶液调节体系的pH值至(3.6)，在50℃水浴中搅拌1.5h，搅拌结束后，采取冰水浴的方法，将体系的温度降至15℃左右，然后用10％的氢氧化钠溶液将体系的pH值调到6.0。
4.固化、清洗：加入0.25％转谷氨酰胺酶，在磁力搅拌器上用较低的转速搅拌，固化10h后获得微胶囊的分散液。将制得的微胶囊分散液静置分层、去上清液，减压过滤，用去离子水水洗得到湿囊，再用无水乙醇洗去湿囊表面未被包埋的三萜类化合物，最后将提取物倒入培养皿中，用保鲜膜封好。
5.冻干：将将上述保鲜膜封好的培养皿放置在DW-HL398型超低温冰箱(中科美菱低温科技股份有限公司)中-80℃下预冻6h，再放到SCIENTZ型真空冷冻干燥机(宁波新芝生物科技股份有限公司)腔体内，设置冷阱温度-30℃左右，真空度在30pa左右，经过冷冻干燥48h后得到粉末状纳米微胶囊。
6.相关指标检测：上述方法制备的杏鲍菇三萜类化合物纳米微胶囊产品的粒径为621.5nm，包埋率达到了78.48％，载药量高达43.95％，微胶囊的微观结构呈球形，表面相对光滑致密且连续，壁材具有较好的完整性和致密性，表明对芯材有良好的保护效果。
具体指标测定方法如下：
①微胶囊粒径测定：将制备的微胶囊溶液均匀搅拌，用移液管吸取少量样品，用粒度分析仪测量微胶囊的粒度分布。
②微观结构观察：采用扫描电子显微镜观察所制得微胶囊粉末的表面形态，并选取具有代表性的视野拍照。
③微胶囊包埋率和载药量测定：在250ml的烧瓶中确切地称量一定质量的干燥好的微胶囊产品，精确加入50ml无水乙醇，在超声清洗器内振荡提取30min。提取后加入无水硫酸钠除去水分，过滤，精确吸取并稀释滤液，测量547nm处的吸光度，并根据标准曲线来计算微胶囊中三萜类化合物的含量。
包埋率(％)＝(包埋进微胶囊中的三萜类化合物的含量/加入的提取物中三萜类化合物的含量)×100
载药量(％)＝(包埋进微胶囊中的三萜类化合物的量/总微胶囊的量)×100
Claims (6)
1.一种杏鲍菇三萜类化合物纳米微胶囊制备方法，其特征是将明胶、海藻酸钠作为壁材，将超声波辅助浸提获得的杏鲍菇三萜类化合物作为芯材，经过芯壁混合、分散、均质、调节温度和pH值、固化、清洗、冻干，获得杏鲍菇三萜类化合物纳米微胶囊。
2.根据权利要求1所述的方法，其特征在于，所述明胶与海藻酸钠比例为1∶1，壁材总浓度为1％-3％，芯壁混合比为1∶1。
3.根据权利要求1所述的方法，其特征在于，所述分散是利用超声波使溶液分散2-4min。所述均质是采用高压微射流均质机在压力10000-13000PSI下对分散溶液进行均质2-4次。
4.根据权利要求1所述的方法，其特征在于，所述调节温度和pH值是先将经过均质的溶液倒入锥形瓶中，加入10％的冰醋酸溶液调节体系的pH值至(3.6)，在50℃水浴中搅拌1.5h，搅拌结束后，采取冰水浴的方法，将体系的温度降到15℃左右，然后用10％的氢氧化钠溶液将体系的pH值调到6.0。
5.根据权利要求1所述的方法，其特征在于，所述固化是加入0.1％-0.3％转谷氨酰胺酶，在磁力搅拌器上用低转速搅拌10-12h获得微胶囊分散液。所述清洗是把制得的微胶囊分散液静置分层，去上清液，减压过滤，用去离子水水洗得到湿囊，再用无水乙醇洗去湿囊表面未被包埋的三萜化合物，将提取物倒入培养皿中，用保鲜膜封好。
6.根据权利要求1所述的方法，其特征在于，所述冻干是在-80～-65℃超低温冰箱下预冻6-8h，再放至真空冷冻干燥腔体内，设置冷阱温度-40℃～-30℃，真空度25-35pa，真空冷冻干燥46-52h。
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