CN107929544B - 白及属植物中militarine部位及单体的制备方法及其应用 - Google Patents
白及属植物中militarine部位及单体的制备方法及其应用 Download PDFInfo
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- CN107929544B CN107929544B CN201711364335.1A CN201711364335A CN107929544B CN 107929544 B CN107929544 B CN 107929544B CN 201711364335 A CN201711364335 A CN 201711364335A CN 107929544 B CN107929544 B CN 107929544B
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- bletilla striata
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Abstract
白及提取物含militarine部位在制备镇静安神、促进睡眠的药物中的应用，白及提取物含militarine部位在制备镇静安神、促进睡眠的功能食品或保健品中的应用，白及提取物含militarine部位在制备美容护肤品中的应用，其中所述白及提取物中militarine含量为25％以上。白及提取物含militarine部位的制备方法，取白及新鲜或干燥药材，粉碎后，以不同浓度乙醇为溶媒提取，蒸去乙醇溶液，水混悬液用大孔树脂柱吸附，先以水洗脱至澄清，再用30％乙醇水洗脱，收集乙醇洗脱液。
Description
技术领域：
本发明属于药物技术领域，具体地，涉及白及属植物中militarine部位及单体的制备方法，以及白及属植物中militarine部位及单体在制备药物、食品、保健品、化妆品中的应用。
背景技术：
白及属(Bletilla Rchb.f)植物是温带地生兰科(Orchidaceae)多年生宿根草本植物，分布于中国、朝鲜半岛、日本等东亚国家。我国该属植物广布于长江流域各省，资源丰富，我国有4种：分别为白及[Bletilla striata(Thunb)Rchb.f.]、小白及[B.formosana(Hayata)Schltr]、黄花白及(B.ochracea Schltr)和华白及[B.sinensis(Rolfe)Schltr]。从1963年至2015年《中国药典》正品白及为兰科植物白及的干燥块茎的干燥根茎。中国西南(尤其是云南)黄花白及和小白及两种植物也作为白及的习用药材。白及药用历史悠久，药用价值明显，具有收敛止血，消肿生肌之功效，临床用于咯血，吐血，外伤出血，疮疡中毒，皮肤皲裂，肺结核咳血及溃疡病出血等病症。现代药理研究显示该属药用植物不仅具有传统功效收敛止血消肿生肌之作用，而且在抗菌及抗癌方面也显示出了新的活性，白及在美容护肤方面也有着广阔的前景。目前，全国以白及为原料的生产厂家超过28家，单方和复方中成药制剂8余个，如白及片，白及胶囊，胃康灵片。
关于白及属化学成分的研究可以追溯到19世纪末，长期以来人们主要集中于正品白及(B.striata)的研究，对同属其它种如小白及(B.formosana)黄花白及(B.ochracea)研究报道较少。1983年日本的Yamaki学者最先对中药白及开展***的化学成分研究，得到了大量菲类衍生物，发现多个具有抗菌活性。90年代以后，我国学者也陆续分离得到一些化学成分。目前，从文献报道，白及属的主要化学成分是联苄(bibenzyls)、菲类(phenanthrenes)及其衍生物、甾体皂苷，三萜，黄酮，花青素等，共150余个。这些成分在后续的研究中表现出多样的生物活性，如抗炎、抗氧化，抗菌、止血、抗肿瘤和抑制络氨酸酶等活性。该属多糖含量丰富，多糖也是其中的功能成分，目前报道的白及多糖骨架类型主要1,2或1,4链接甘露糖残基与葡萄糖残基1,4链接方式。药理活性研究白及多糖具有抑制血管内皮细胞的增长繁殖，抑制血管紧缩素Ⅱ诱发血管内ROS和炎症通过TLR2通路，刺激脾脏细胞的增殖，抗纤维等活性。此外白及多糖也称白及胶是重要的生物材料，作为加工***、血管栓塞剂用于肿瘤的介入疗。
发明内容：
本发明的目的在于提供白及属植物中militarine部位及单体的制备方法，以及白及属植物中militarine部位及单体在制备药物、食品、保健品、化妆品中的应用。更进一步地，提供白及属植物中militarine部位及单体在制备镇静安神、促进睡眠的药物、保健品、食品中的应用，以及在制备美容护肤品中的应用。
为了实现本发明的上述目的，本发明提供了如下的技术方案：
白及提取物含militarine部位在制备镇静安神、促进睡眠的药物中的应用，其中所述白及提取物中militarine含量为25％以上。
白及提取物含militarine部位在制备镇静安神、促进睡眠的功能食品或保健品中的应用，其中所述白及提取物中militarine含量为25％以上。
白及提取物含militarine部位在制备美容护肤品中的应用，其中所述白及提取物中militarine含量为25％以上。
根据所述的应用，所述的白及提取物含militarine部位由下述方法制备而得：白及新鲜或干燥药材，进行粉碎后，以乙醇∶水0％-95％为溶媒提取，蒸去乙醇溶液，水混悬液以正己烷或乙酸乙酯脱脂处理后再用正丁醇萃取，所得正丁醇萃取液浓缩干燥后得主含militarine部位，正丁醇萃取物中militarine的含量大于25％。
根据所述的应用，所述的白及提取物含militarine部位由下述方法制备而得：取干白及块茎粉末，按1:4加80％乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏，用热水溶解浸膏，水混悬液1:3乙酸乙酯萃取脱脂，再用1:1正丁醇萃取，重复萃取3次，合并3次滤液，得浸膏，正丁醇萃取物中militarine的含量大于25％。
根据所述的应用，所述的白及提取物含militarine部位由下述方法制备而得：取干白及块茎粉末，按1:4加80％乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏；用热水充分搅拌溶解并稀释浸膏，所得水液用大孔树脂柱吸附，先以水洗脱至澄清，再用30％乙醇水洗脱，收集乙醇洗脱液，减压回收乙醇得到产物浸膏，浸膏中militarine的含量大不超过25％。
白及提取物含militarine部位的制备方法，取白及新鲜或干燥药材，粉碎后，以乙醇∶水为0％-95％为溶媒提取，蒸去乙醇溶液，水混悬液用大孔树脂柱吸附，先以水洗脱至澄清，再用30％乙醇水洗脱，收集乙醇洗脱液，得到主含militarine部位。
根据所述的白及提取物含militarine部位的制备方法，其中使用的大孔吸附树脂柱为D101、LX-17。
化合物militarine在制备镇静安神、促进睡眠的药物、保健品、功能食品中的应用。
化合物militarine在制备美容护肤品中的应用，
与现有技术相比，本发明的优益性在于：
虽然中国药典一部未界定白及药材的含量测定指标，本发明的研究与多样本分析表明，militarine在白及干药材中的含量平均达到2％以上，易于富集与产业化生产。Militarine是苄醇酯苷类成分，与现有技术从天麻中获取苄醇酯苷类成分部位相比较，从白及中制备militarine更经济高效，而且成分单一，易于产业化与质控。
附图说明：
图1.militraine标准品HPLC图谱；
图2.正丁醇萃取HPLC图谱；
图3.30％乙醇洗脱物HPLC图谱；
图4militarine及天麻素组对小鼠体重变化图；
图5 M2组给药10min后小鼠入睡情况；
图6 G2组给药10min后小鼠入睡情况。
具体实施方式：
下面结合附图，用本发明的实施例来进一步说明本发明的实质性内容，但并不以此来限定本发明。
实施例1：
取干白及块茎粉末1000g，按1:4加80％乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏，用热水溶解浸膏，水混悬液1:3乙酸乙酯萃取脱脂，再用1:1正丁醇萃取，重复萃取3次，合并3次滤液，得到80g浸膏。经HPLC检测分析，表明正丁醇萃取物中的主要成分为militarine，与militarine标准对照品采用外标法进行含量分析，检测正丁醇萃取物中militarine的含量为28.0％。
将militarine正丁醇萃取部位80克，用凝胶柱LH-20分离，乙醇洗脱，得到militarine单体化合物20.5克。
化合物militarine，具有如下理化特征：
分子式：C34H46O17
分子量：726
英文名：militarine
化学结构：
实施例2：
取干白及块茎粉末1000g，按1:4加80％乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏；用热水充分搅拌溶解并稀释浸膏，所得水液用大孔树脂柱吸附，先以水洗脱至澄清，再用乙醇30％乙醇水洗脱，收集乙醇洗脱液，减压回收乙醇得到产物浸膏82g；经HPLC检测分析，表明产物浸膏中的主要成分为militarine，与militarine标准对照品采用外标法进行含量分析，检测产物浸膏中militarine的含量为32.0％。
将富含militarine洗脱浸膏部位82克，用凝胶柱LH-20分离，乙醇洗脱，得到militarine单体化合物24.5克。
实施例3：
小鼠体内镇静助眠实验：
1、实验材料与方法
1.1、药品与试剂
militarine为实验室制备所获得的供试样品,天麻素，戊巴比妥钠，腺苷，GABA，L-谷氨酸，多巴胺，去甲肾上腺素，生理盐水。
1.2、实验动物
清洁级Balb/c小鼠，雄性，体重，20±2g，由南京鹏晟生物科技发展有限公司供给，许可证号为SCXK(苏)2016-0010。实验条件下自然饮食，适应环境五天后进行实验。
1.3、仪器和设备
小鼠自主活动仪，分析天平，高效液相色谱仪，超声波清洁仪，超净工作台。
1.4、溶液配制
将40mg的militarine溶于生理盐水中，配成10mg/ml的试剂；80mg的militarine溶于生理盐水中，配成20mg/ml的试剂；将40mg的天麻素溶于生理盐水中，配成10mg/ml的试剂；80mg的天麻素溶于生理盐水中，配成20mg/ml的试剂；50mg的戊巴比妥钠溶于生理盐水中，配成10mg/ml的试剂
2、实验方法
2.1、实验动物分组及给药
Balb/c雄性小鼠53只，随机分为10组，每组5-6只；分组及给药剂量如(表1)。
表1实验动物分组及给药(ip,8d)
2.2对阈下剂量戊巴比妥钠致小鼠睡眠时间的影响
观察各组药物能否延长戊巴比妥钠所致睡眠时间。正式实验前进行预实验，确定阈下戊巴比妥钠剂量为50mg/kg。于末次注射给药后同时腹腔注射戊巴比妥钠(50mg/kg)，以翻正反射消失1min为入睡时间，即潜伏期。从翻正反射消失致恢复时间为睡眠时间。
2.3小鼠自主活动测试
末次腹腔注射给予相应药物10min后将小鼠放入自主活动箱内，以计算机输出5分钟内小鼠切断箱内光束的次数作为小鼠的自主活动次数。
3、实验结果与分析
3.1药物对小鼠体重的影响
给药期间，小鼠体重变化情况(图4)：Blank，M1，M2，M3组及阳性对照G1，G2，G3，G4组小鼠体重成递增趋势；Control阴性及给药M4组小鼠体重保持平稳；研究表明研究的militarine及天麻素对小鼠体重无毒副作用。
3.2对小鼠自主活动的影响
militarine组及天麻素组对小鼠自主活动的影响，结果见表2。各实验组对小鼠活动次数未见显著性差异，M2，M4组(militarine低，高剂量协同戊巴比妥钠组)和Control(戊巴比妥钠阈下剂量组)组对小鼠站立次数与空白对照组有极显著性差异(P＜0.01)，阳性对照G2和G4组(天麻素低，高剂量协同戊巴比妥钠组)与空白对照组有显著性差异(P＜0.05)。
表2 militarine及天麻素组对小鼠自主活动的影响(X±S)
注：*与对空白组比较P＜0.05，**与空白组比较P＜0.01。
3.3对小鼠睡眠的影响
militarine及天麻素组对小鼠睡眠的作用，结果见表3，图5,6。由表中可见，与空白对照组比较，药物组M2和M4组能明显延长小鼠睡眠的时间(P＜0.01，P＜0.05)，阳性对照G2能延长小鼠睡眠的时间(P＜0.01，P＜0.05)。
表3 militarine及天麻素组对小鼠睡眠的影响(X±S)
注：*与对空白组比较P＜0.05，**与空白组比较P＜0.01。
实施例4：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，分别按常规加注射用水，精滤，灌封灭菌制成注射液。
实施例5：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，分别将其溶于无菌注射用水中，搅拌使溶，用无菌抽滤漏斗过滤，再无菌精滤，分装于2安瓿中，低温冷冻干燥后无菌熔封得粉针剂。
实施例6：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，分别与赋形剂重量比为9:1的比例加入赋形剂，制成粉剂。
实施例7：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，，分别按其与赋形剂重量比为1:5–1:10的比例加入赋形剂，制粒压片。
实施例8：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，，分别按常规口服液制法制成口服液。
实施例9：
按实施例1的方法先制得白及正丁醇萃取物，及化合物militarine，，分别按其与赋形剂重量比为3:1的比例加入赋形剂，制成胶囊或颗粒剂或冲剂。
实施例10：
按实施例1的方法制得白及正丁醇萃取物，及化合物militarine 12.4克，分别加入淀粉600克，乳糖200克，薄荷醇5克，羧甲基淀粉钠183克，制成含片，作为功能食品。
Claims (3)
1.白及提取物含militarine部位在制备镇静安神、促进睡眠的药物中的应用，其中所述白及提取物中militarine含量为25%以上，所述的白及提取物含militarine部位由下述方法制备而得：
取干白及块茎粉末，按质量比1:4加80%乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏，用热水溶解浸膏，水混悬液1:3乙酸乙酯萃取脱脂，再用1:1正丁醇萃取，重复萃取3次，合并3次滤液，得浸膏，正丁醇萃取物中militarine的含量大于25%；
或由下述方法制备而得：取干白及块茎粉末，按1:4加80%乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏；用热水充分搅拌溶解并稀释浸膏，所得水液用大孔树脂柱吸附，先以水洗脱至澄清，再用30%乙醇水洗脱，收集乙醇洗脱液，减压回收乙醇得到产物浸膏，浸膏中militarine的含量超过25 %。
2.白及提取物含militarine部位在制备镇静安神、促进睡眠的功能食品中的应用，其中所述白及提取物中militarine含量为25%以上，所述的白及提取物含militarine部位由下述方法制备而得：
取干白及块茎粉末，按质量比1:4加80%乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏，用热水溶解浸膏，水混悬液1:3乙酸乙酯萃取脱脂，再用1:1正丁醇萃取，重复萃取3次，合并3次滤液，得浸膏，正丁醇萃取物中militarine的含量大于25%；
或由下述方法制备而得：取干白及块茎粉末，按1:4加80%乙醇，在90℃下回流提取180min，冷却至室温，抽滤，重复再提取2次，合并3次滤液，减压浓缩回收乙醇，得白及块茎粗提物浸膏；用热水充分搅拌溶解并稀释浸膏，所得水液用大孔树脂柱吸附，先以水洗脱至澄清，再用30%乙醇水洗脱，收集乙醇洗脱液，减压回收乙醇得到产物浸膏，浸膏中militarine的含量超过25 %。
3.化合物militarine在制备镇静安神、促进睡眠的药物、功能食品中的应用。
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