CN106667937A - 一种黑枸杞多糖咀嚼片 - Google Patents
一种黑枸杞多糖咀嚼片 Download PDFInfo
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- CN106667937A CN106667937A CN201710002997.8A CN201710002997A CN106667937A CN 106667937 A CN106667937 A CN 106667937A CN 201710002997 A CN201710002997 A CN 201710002997A CN 106667937 A CN106667937 A CN 106667937A
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- lycium ruthenicum
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- 241000169546 Lycium ruthenicum Species 0.000 title claims abstract description 62
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2054—Cellulose; Cellulose derivatives, e.g. hydroxypropyl methylcellulose
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0053—Mouth and digestive tract, i.e. intraoral and peroral administration
- A61K9/0056—Mouth soluble or dispersible forms; Suckable, eatable, chewable coherent forms; Forms rapidly disintegrating in the mouth; Lozenges; Lollipops; Bite capsules; Baked products; Baits or other oral forms for animals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
-
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
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- A61K2236/30—Extraction of the material
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/30—Extraction of the material
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- A—HUMAN NECESSITIES
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- 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)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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Abstract
本发明涉及一种黑枸杞多糖咀嚼片，其主要成分包括黑枸杞多糖、甘露醇、枸橼酸糖浆、羟丙基纤维素、聚维酮K30和微粉硅胶，本发明对黑枸杞进行热水浸提，采用石油醚萃取进行脱脂脱色素，更大程度地去除杂质并保留更多的多糖成分，醇沉后再经凝胶柱层析进行纯化精制，药效更为集中，充分发挥了黑枸杞多糖的药理活性。所述咀嚼片具有较好的口感，崩解时间短、分散效果好、药物溶出迅速、吸收快、生物利用度高等优点。服用方便，尤其适合儿童、老人、吞咽困难的患者服用。
Description
技术领域
本发明涉及一种黑枸杞多糖咀嚼片，属于功能食品领域。
背景技术
黑枸杞，又称黑果枸杞，系茄科枸杞属。多年生灌木，具棘刺，浆果球形，成熟后为紫黑色，有很高的光合效率和较强抗逆性，是我国西北荒漠地区一种特有的亟待开发的野生植物，分布于山西、宁夏、甘肃、青海、新疆、西藏等地区。黑枸杞味甜多汁，含丰富的维生素、有机酸及糖类，民间常生食或榨汁做饮料。黑枸杞具有一定的医疗保健功能，藏医用它治疗心热病、心脏病、月经不调、停经等病症。
黑枸杞中富含蛋白质、脂肪、糖类、游离氨基酸、有机酸、矿物质、微量元素、生物碱、维生素C、B1、B2、钙、镁、铜、锌、锰、铁、铅、镍、镉、钴、铬、钾、钠等各种营养成分。目前，对黑枸杞活性成分研究最多的是黑枸杞中富含的花色苷类色素和多糖类。现代药理研究表明，黑枸杞花色苷类色素具有显著的抗氧化和抗衰老等活性，黑枸杞多糖具有抗疲劳、降血糖等活性。
随着近年来黑枸杞保健食品的开发，黑枸杞产品不再拘泥于果汁、果酒、果粉等形式。不断涌现的新型保健食品包括：将黑枸杞制成口服液等形式、与红枸杞或其它具有保健功效的药食同源类药材(如绞股蓝、红景天等)制成功能食品、或者提取出黑枸杞中的花色苷类(如原花青素等)制成泡腾片、口含片等形式。
目前，对黑枸杞多糖的研究大多集中于提取方法/工艺的研究、药理活性的研究等，缺少涉及黑枸杞多糖作为单一活性成分的功能保健食品。
发明内容
为丰富黑枸杞多糖的功能食品类型，本发明的一个目的是提供一种黑枸杞多糖咀嚼片，其主要成分包括：黑枸杞多糖40-60g，甘露醇240-300g，枸橼酸糖浆6-9g，羟丙基纤维素10-15g，聚维酮K30 20-30g，微粉硅胶4-6g。
在一个实施方案中，所述咀嚼片的主要成分包括：黑枸杞多糖45g，甘露醇250g，枸橼酸糖浆8g，羟丙基纤维素12g，聚维酮K30 24g，微粉硅胶5g。
在一个实施方案中，黑枸杞多糖的制备方法包括以下步骤：
(1)挑选优质的黑枸杞，用净水清洗，烘干，粉碎成粗粉备用；
(2)将步骤(1)所得的黑枸杞粗粉经热水浸提2-3次，每次1.5-2.5h，合并所得浸提液，过滤，浓缩至原体积的二分之一；
(3)将步骤(2)所得浓缩液中加入1-2倍体积的石油醚萃取，萃取2-4次，弃去石油醚萃取层，合并萃取后的水层备用；
(4)将步骤(3)中所得水层中加入适量水，将水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置12-24h，抽滤，沉淀备用，将抽滤后所得水层减压浓缩至乙醇完全挥去，加入适量至水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置12-24h，抽滤，合并两次所得沉淀物，用无水乙醇洗涤2-3次，干燥，备用；
(5)将步骤(4)中所得的沉淀，加少量水溶解后，经凝胶色谱柱进行纯化，洗脱液为0.1-0.15mol/L的NaCl水溶液，将收集的洗脱液浓缩、透析脱盐，干燥，即得经纯化的黑枸杞多糖。
在一个实施方案中，所述的凝胶色谱柱是Sephadex G-100凝胶色谱柱。
在一个实施方案中，所述咀嚼片的制备方法包括以下步骤：
(1)分别按比例称取黑枸杞多糖和甘露醇，过40目筛，过筛后混合均匀，备用；
(2)将羟丙基纤维配制成1.5-2％的水溶液，加入至步骤(1)所得的混合物料中制成软材，将所得软材制粒，过16-20目筛，烘干，整粒；
(3)按比例取聚维酮K30和微粉硅胶，与步骤(2)所得颗粒混合均匀，最后按比例加入枸橼酸糖浆混合均匀，压片，即得所述咀嚼片。
有益效果：
(1)本发明的黑枸杞多糖咀嚼片具有较好的口感，崩解时间短、分散效果好、药物溶出迅速并且稳定性佳。
(2)本发明对黑枸杞进行热水浸提，采用石油醚萃取进行脱脂脱色素，更大程度地去除杂质并保留更多的多糖成分，醇沉后再经凝胶柱层析进行纯化精制，药效更为集中，充分发挥了黑枸杞多糖的药理活性，还具有吸收快、生物利用度高的优点。同时，服用方便，尤其适合儿童、老人、吞咽困难的患者服用。
具体实施方式
还可进一步通过实施例来理解本发明，其中所述实施例说明了一些制备或使用方法。然而，要理解的是，这些实施例不限制本发明。现在已知的或进一步开发的本发明的变化被认为落入本文中描述的和以下要求保护的本发明范围之内。
实施例1
一种黑枸杞多糖咀嚼片，主要成分包括：黑枸杞多糖45g，甘露醇250g，枸橼酸糖浆8g，羟丙基纤维素12g，聚维酮K30 24g，微粉硅胶5g；其制备方法包括如下步骤：
(1)黑枸杞多糖的制备：
(a)挑选优质的黑枸杞，用净水清洗，烘干，粉碎成粗粉备用；
(b)将步骤(a)所得的黑枸杞粗粉经热水浸提3次，每次2h，合并所得浸提液，过滤，浓缩至原体积的二分之一；
(c)将步骤(b)所得浓缩液中加入2倍体积的石油醚萃取，萃取4次，弃去石油醚萃取层，合并萃取后的水层备用；
(d)将步骤(c)中所得水层中加入适量水，将水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置18h，抽滤，沉淀备用，将抽滤后所得水层减压浓缩至乙醇完全挥去，加入适量至水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置18h，抽滤，合并两次所得沉淀物，用无水乙醇洗涤3次，干燥，备用；
(e)将步骤(d)中所得的沉淀，加少量水溶解后，经凝胶色谱柱进行纯化，洗脱液为0.1mol/L的NaCl水溶液，将收集的洗脱液浓缩、透析脱盐，干燥，即得经纯化的黑枸杞多糖。
(2)咀嚼片的制备：
(a)分别按比例称取黑枸杞多糖和甘露醇，过40目筛，过筛后混合均匀，备用；
(b)将羟丙基纤维配制成1.5％的水溶液，加入至步骤(1)所得的混合物料中制成软材，将所得软材制粒，过20目筛，烘干，整粒；
(c)按比例取聚维酮K30和微粉硅胶，与步骤(2)所得颗粒混合均匀，最后按比例加入枸橼酸糖浆混合均匀，压片，即得所述咀嚼片。
实施例2
一种黑枸杞多糖咀嚼片，主要成分包括：黑枸杞多糖50g，甘露醇270g，枸橼酸糖浆8g，羟丙基纤维素10g，聚维酮K30 25g，微粉硅胶6g；其制备方法包括如下步骤：
(1)黑枸杞多糖的制备：
(a)挑选优质的黑枸杞，用净水清洗，烘干，粉碎成粗粉备用；
(b)将步骤(a)所得的黑枸杞粗粉经热水浸提2次，每次2.5h，合并所得浸提液，过滤，浓缩至原体积的二分之一；
(c)将步骤(b)所得浓缩液中加入1.5倍体积的石油醚萃取，萃取3次，弃去石油醚萃取层，合并萃取后的水层备用；
(d)将步骤(c)中所得水层中加入适量水，将水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置24h，抽滤，沉淀备用，将抽滤后所得水层减压浓缩至乙醇完全挥去，加入适量至水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置20h，抽滤，合并两次所得沉淀物，用无水乙醇洗涤3次，干燥，备用；
(e)将步骤(d)中所得的沉淀，加少量水溶解后，经凝胶色谱柱进行纯化，洗脱液为0.15mol/L的NaCl水溶液，将收集的洗脱液浓缩、透析脱盐，干燥，即得经纯化的黑枸杞多糖。
(2)咀嚼片的制备：
(a)分别按比例称取黑枸杞多糖和甘露醇，过40目筛，过筛后混合均匀，备用；
(b)将羟丙基纤维配制成2％的水溶液，加入至步骤(1)所得的混合物料中制成软材，将所得软材制粒，过16目筛，烘干，整粒；
(c)按比例取聚维酮K30和微粉硅胶，与步骤(2)所得颗粒混合均匀，最后按比例加入枸橼酸糖浆混合均匀，压片，即得所述咀嚼片。
实施例3
一种黑枸杞多糖咀嚼片，主要成分包括：黑枸杞多糖60g，甘露醇300g，枸橼酸糖浆9g，羟丙基纤维素15g，聚维酮K30 30g，微粉硅胶6g其制备方法包括如下步骤：
(1)黑枸杞多糖的制备：
(a)挑选优质的黑枸杞，用净水清洗，烘干，粉碎成粗粉备用；
(b)将步骤(a)所得的黑枸杞粗粉经热水浸提3次，每次2.5h，合并所得浸提液，过滤，浓缩至原体积的二分之一；
(c)将步骤(b)所得浓缩液中加入2倍体积的石油醚萃取，萃取3次，弃去石油醚萃取层，合并萃取后的水层备用；
(d)将步骤(c)中所得水层中加入适量水，将水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置24h，抽滤，沉淀备用，将抽滤后所得水层减压浓缩至乙醇完全挥去，加入适量至水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置24h，抽滤，合并两次所得沉淀物，用无水乙醇洗涤3次，干燥，备用；
(e)将步骤(d)中所得的沉淀，加少量水溶解后，经凝胶色谱柱进行纯化，洗脱液为0.1mol/L的NaCl水溶液，将收集的洗脱液浓缩、透析脱盐，干燥，即得经纯化的黑枸杞多糖。
(2)咀嚼片的制备：
(a)分别按比例称取黑枸杞多糖和甘露醇，过40目筛，过筛后混合均匀，备用；
(b)将羟丙基纤维配制成2％的水溶液，加入至步骤(1)所得的混合物料中制成软材，将所得软材制粒，过20目筛，烘干，整粒；
(c)按比例取聚维酮K30和微粉硅胶，与步骤(2)所得颗粒混合均匀，最后按比例加入枸橼酸糖浆混合均匀，压片，即得所述咀嚼片。
实施例4片剂指标测定
(1)片剂硬度测定
取实施例1制得的咀嚼片15片，按照药典中规定的硬度测定法，测定咀嚼片的硬度，测得平均值为3.5kg/cm2。
(2)片重差异
取实施例1制得的咀嚼片30片，精密称取总质量，计算得出平均片重，每片片重与平均片重相比，均未超过质量差异±2.2％。
(3)脆碎度
取实施例1制得的咀嚼片20片，按药典规定的脆碎度方法进行测定，试验前20片片重与试验后20片质量相比较，失重为0.35％。
从以上试验可以看出，本发明制得的咀嚼片完全符合药典规定。
实施例5 稳定性考察
将制备的咀嚼片置于45℃和75％湿度环境下放置了六个月，然后取出咀嚼片研细，加水超声提取二次，每次30min，过滤合并滤液；按照硫酸苯酚法测定咀嚼片中多糖含量(放置后多糖含量/放置前多糖含量×100％)，具体结果如下：
| 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | |
| 3个月 | 99.7％ | 98.2％ | 97.4％ | 92.1％ | 94.8％ |
| 6个月 | 99.2％ | 95.6％ | 94.1％ | 86.8％ | 85.3％ |
对比例1的制备方法同实施例1，区别仅在于制备过程中将辅料羟丙基纤维素替换为等量的聚维酮K30
对比例2的制备方法同实施例1，区别仅在于制备过程中将辅料聚维酮K30替换为等量的羟丙基纤维素
本发明内容仅仅举例说明了要求保护的一些具体实施方案，其中一个或更多个技术方案中所记载的技术特征可以与任意的一个或多个技术方案相组合，这些经组合而得到的技术方案也在本申请保护范围内，就像这些经组合而得到的技术方案已经在本发明公开内容中具体记载一样。
Claims (5)
1.一种黑枸杞多糖咀嚼片，其特征在于，其主要成分包括：黑枸杞多糖40-60g，甘露醇240-300g，枸橼酸糖浆6-9g，羟丙基纤维素10-15g，聚维酮K30 20-30g，微粉硅胶4-6g。
2.根据权利要求1所述的咀嚼片，其特征在于，其主要成分包括：黑枸杞多糖45g，甘露醇250g，枸橼酸糖浆8g，羟丙基纤维素12g，聚维酮K30 24g，微粉硅胶5g。
3.根据权利要求1所述的咀嚼片，其特征在于，所述黑枸杞多糖的制备方法包括以下步骤：
(1)挑选优质的黑枸杞，用净水清洗，烘干，粉碎成粗粉备用；
(2)将步骤(1)所得的黑枸杞粗粉经热水浸提2-3次，每次1.5-2.5h，合并所得浸提液，过滤，浓缩至原体积的二分之一；
(3)将步骤(2)所得浓缩液中加入1-2倍体积的石油醚萃取，萃取2-4次，弃去石油醚萃取层，合并萃取后的水层备用；
(4)将步骤(3)中所得水层中加入适量水，将水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置12-24h，抽滤，沉淀备用，将抽滤后所得水层减压浓缩至乙醇完全挥去，加入适量至水层中的沉淀完全溶解，再加入浓度为95％的乙醇直至乙醇浓度降至50％，低温静置12-24h，抽滤，合并两次所得沉淀物，用无水乙醇洗涤2-3次，干燥，备用；
(5)将步骤(4)中所得的沉淀，加少量水溶解后，经凝胶色谱柱进行纯化，洗脱液为0.1-0.15mol/L的NaCl水溶液，将收集的洗脱液浓缩、透析脱盐，干燥，即得经纯化的黑枸杞多糖。
4.根据权利要求3所述的咀嚼片，其特征在于，步骤(5)中，所述凝胶色谱柱是SephadexG-100凝胶色谱柱。
5.根据权利要求1所述的咀嚼片，其特征在于，所述咀嚼片的制备方法包括以下步骤：
(1)分别按比例称取黑枸杞多糖和甘露醇，过40目筛，过筛后混合均匀，备用；
(2)将羟丙基纤维配制成1.5-2％的水溶液，加入至步骤(1)所得的混合物料中制成软材，将所得软材制粒，过16-20目筛，烘干，整粒；
(3)按比例取聚维酮K30和微粉硅胶，与步骤(2)所得颗粒混合均匀，最后按比例加入枸橼酸糖浆混合均匀，压片，即得所述咀嚼片。
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