CN108635361B - 一种具有抗炎活性的琼花提取物及其活性成分和分离方法 - Google Patents
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Abstract
本发明公开了一种具有抗炎活性的琼花提取物及其活性成分和该活性成分的提取分离方法,以及该活性成分在抗炎方面的应用,所述琼花提取物是以体积百分数为70%至95%的乙醇水溶液为提取剂对琼花地上干燥部分进行回流提取,所得提取液即为所述琼花提取物;通过对所述琼花提取物进行处理,提取分离出两种抗炎活性成分,即3‑羟基‑4‑(6‑苯甲酰基‑β‑D‑吡喃葡萄糖基)苯甲酸苯甲酯和4‑羟基‑3‑(6‑肉桂酰基‑β‑D‑吡喃葡萄糖基)苯甲酸苯甲酯,上述琼花提取物和两种化合物均表现出明显的抗炎作用,能够在制药、食品及保健品领域应用。
Description
技术领域
本发明涉及一种具有抗炎活性的琼花提取物及其活性成分和分离方法,属于琼花抗炎活性成分提取分离技术领域。
背景技术
琼花(拉丁学名:Viburnum macrocephalum Fort.f.keteleeri)为荚蒾属植物。琼花又称聚八仙、蝴蝶花,属于绣球荚蒾的变种,为我国特有的名贵花木。琼花是扬州市花和昆山三宝之一,为忍冬科半常绿灌木。春季其花大如盘、洁白如玉;秋季果实累累、红绿相间,是极具观赏价值的园林植物。近年来以扬州瘦西湖、昆山亭林园为源头,琼花得以大规模繁殖,已经成为道路绿化、公园景观以及小区绿化的特色树种。在民间,琼花常以枝、叶、果入药,具有通经活络、解毒止痒之功效,一般春夏采摘,晒干可用。茎煎水可治风湿疥癣,皮肤痒痛,内服外用均可;花泡酒,可治跌打损伤。
国内外对其药学应用的物质基础研究尚不多见,截至目前,文献报道的仅见从琼花中分离得到的8个黄酮类化合物。
发明内容
发明目的:针对上述技术问题,本发明提供了一种具有抗炎活性的琼花提取物及其活性成分和分离方法,该琼花提取物以及所得两种活性成分,均可以作为炎症治疗药物,以及炎症为并发症的各种重大疾病的辅助治疗药物、食品及保健品。
技术方案:为了达到上述发明目的,本发明所采用的技术方案如下:
一种具有抗炎活性的琼花提取物,以体积百分数为70%至95%的乙醇水溶液为提取剂对琼花地上干燥部分进行回流提取,所得提取液即为所述琼花提取物。
上述回流提取时,料液比为1:(4-6),提取次数为2-4次,每次提取时间为1-3h。
一种所述琼花提取物中的抗炎活性成分,其为3-羟基苯甲酸苯甲酯类化合物,化学结构式如下所示:
化合物1:3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯,分子式为C27H26O10,分子量为510.1526。
另一种所述琼花提取物中的抗炎活性成分,其为4-羟基苯甲酸苯甲酯类化合物,化学结构式如下所示:
化合物2:4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯,分子式为C29H28O10,分子量为536.1682。
本发明上述提取物和化合物均表现出明显的抗炎作用。作为植物提取物,可作为抗炎药物应用于炎症治疗及炎症为并发症的各种重大疾病的辅助治疗药物、食品及保健品领域。本发现丰富了对琼花中次生代谢产物的认识,为琼花在药品、食品及保健品领域应用的开发、合理应用及深入研究提供科学依据。
上述3-羟基苯甲酸苯甲酯类化合物和4-羟基苯甲酸苯甲酯类化合物的提取方法,包括以下步骤:
(1)采用乙醇的水溶液对琼花地上部位进行回流提取,通过减压回收溶剂,对提取液进行浓缩干燥,取得浸膏,将浸膏溶解于蒸馏水中,采用乙酸乙酯进行萃取,取得乙酸乙酯萃取液,此萃取液进行减压浓缩后,获得乙酸乙酯萃取浸膏;
(2)乙酸乙酯萃取浸膏上样于MCI微孔树脂色谱柱,以体积百分数为80%至90%的甲醇水溶液为流动相,进行洗脱,收集此流动相的洗脱物,减压浓缩得到流分A;
(3)将流分A上样于硅胶柱色谱,先后以体积比为100:4和100:8的氯仿和甲醇混合液为流动相,进行洗脱,分别收集洗脱物,得到两个流分,流分A-1和流分A-2;
(4)流分A-2经Sephadex LH-20柱色谱进行分离,以体积百分数为55%至60%的甲醇水溶液为流动相,经Sephadex LH-20柱色谱进行梯度洗脱,收集此流动相的洗脱物,减压浓缩得流分A-2-1;
(5)流分A-2-1经ODS柱色谱进行分离,以体积百分数为40%至65%的甲醇水溶液为流动相进行梯度洗脱,收集此流动相的洗脱物,减压浓缩取得流分A-2-1-1和流分A-2-1-2;
流分A-2-1-1经鉴定,即为所述化合物1:3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯。
流分A-2-1-2经鉴定,即为所述化合物2:4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯。
所述步骤(1)中浓缩干燥的温度为40℃。
步骤(2)中所述的乙酸乙酯萃取浸膏先用体积百分数为80%至90%的甲醇水溶液溶解,然后再上样。
本发明的提取分离工艺特点如下:采用一定浓度的乙醇-水溶液对药材进行提取---乙酸乙酯萃取结合MCI微孔树脂富集目标化合物---硅胶、Sephadex LH-20和ODS柱色谱法进行细化分离。通过这一流程,能够最大可能富集琼花中连接单糖的酚苷类次生代谢产物。通过乙酸乙酯萃取除去多糖等强极性化合物,通过MCI微孔树脂去除脂肪酸及叶绿素等小极性化合物,最后依据化合物的结构和极性的差异,通过硅胶、Sephadex LH-20和ODS柱色谱方法进一步将3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯和4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯纯化出来。
本发明还提供了一种组合物,该组合物包含所述琼花提取物、所述3-羟基苯甲酸苯甲酯类化合物和/或所述4-羟基苯甲酸苯甲酯类化合物,以及药学、食品及保健品可接受的载体或赋形剂。
所述药学、食品及保健品可接受的载体或赋形剂选自稀释剂、分散剂、助悬剂、表面活性剂、等渗剂、增稠剂、乳化剂、防腐剂、粘合剂、润滑剂、稳定剂、水合剂、乳化加速剂、缓冲剂、吸收剂、着色剂、香味剂、甜味剂、离子交换剂、脱模剂、涂布剂、矫味剂、和抗氧化剂等。
本发明最后提供了所述琼花提取物、所述3-羟基苯甲酸苯甲酯类化合物或所述4-羟基苯甲酸苯甲酯类化合物在制备抗炎药物、食品或保健品中的应用。其作为抗炎药物、食品或保健品,可以应用于炎症治疗,以及炎症为并发症的各种重大疾病的辅助治疗。
技术效果:相对于现有技术,本发明首次提出了从琼花乙醇提取物的乙酸乙酯萃取部分分离得到新化合物,并且通过乙醇-水溶液对药材进行提取---乙酸乙酯萃取结合MCI微孔树脂富集目标化合物---硅胶、Sephadex LH-20和ODS柱色谱法进行细化分离,从而能够最大可能富集该化合物;所得化合物表现出明显的抗炎作用,可用于炎症治疗及炎症为并发症的各种重大疾病的辅助治疗药物、食品及保健品。
附图说明
图1为本发明化合物的正离子高分辨质谱图,其中A为化合物1,B为化合物2;
图2为本发明化合物的红外图,其中A为化合物1,B为化合物2;
图3为本发明化合物的紫外图,其中A为化合物1,B为化合物2;
图4为本发明化合物的HSQC图(1H的异核单量子相干相关谱,即1H核与其直接相连的13C相关联),其中A为化合物1,B为化合物2;
图5为本发明化合物的HMBC图[1H的异核多键相关谱。突出表现1H核与相隔2个键(2JCH)和相隔3个键(3JCH)的13C相关联],其中A为化合物1,B为化合物2。
具体实施方式
下面通过具体实施例对本发明所述的技术方案给予进一步详细的说明,但有必要指出以下实施例只用于对发明内容的描述,并不构成对本发明保护范围的限制。
实施例
一.使用的仪器与材料:
1.Bruker AVANCE-600型核磁共振波谱仪(德国),Bruker MaXis超高分辨飞行时间质谱仪(德国)。Heal Force HF90CO2培养箱(中国济南);Thermo Multiskan GO全波长酶标仪(美国)
2.MCI微孔树脂:由日本三菱公司生产;Sephadex LH-20:由美国GE公司生产销售;柱层析硅胶:200-300目,由中国青岛海洋化工公司生产销售;ODS:由日本YMC生产。
高效硅胶板GF254:由中国青岛海洋化工公司生产销售;色谱试剂均为分析纯。
3.琼花采自江苏省扬州市,并由扬州大学生物科学与技术学院淮虎银教授鉴定为琼花(Viburnum macrocephalum Fort.f.keteleeri),留样标本(20131005)存放在扬州大学生物科学与技术学院。
二.琼花提取物制备:
1.取1.0kg琼花干燥地上部分,以体积百分数为70%的乙醇为提取溶剂,料液比为1:5,回流提取三次,每次2h。合并提取液,即得所述琼花提取物;
2.取1.0kg琼花干燥地上部分,以体积百分数为85%的乙醇为提取溶剂,料液比为1:4,回流提取4次,每次1h。合并提取液,即得所述琼花提取物;
3.取1.0kg琼花干燥地上部分,以体积百分数为95%的乙醇为提取溶剂,料液比为1:5,回流提取2次,每次3h。合并提取液,即得所述琼花提取物;
三、抗炎活性成分分离:
1、将上述琼花提取物制备项所得琼花提取物在40℃下减压浓缩,得约250g浸膏。将250g浸膏溶解于1L蒸馏水后,用等体积乙酸乙酯进行萃取,取得乙酸乙酯层萃取液。萃取液减压浓缩后得到浸膏35g。
2.将35g乙酸乙酯萃取浸膏溶于300mL体积百分数为80%至90%的甲醇水溶液中,300mL乙酸乙酯萃取物溶液上样于MCI微孔树脂色谱柱,以体积百分数为80%至90%的甲醇水溶液300mL作为流动相进行洗脱,收集洗脱液后减压浓缩得29g流分A。
3.取流分A,将29g浸膏加入58g柱层析硅胶拌样,经100至200g硅胶柱色谱分离。其中色谱分离的流动相依次采用体积比为100:4和100:8的氯仿和甲醇混合液。洗脱液经薄层色谱分析。最终,洗脱液分为2个流分:流分A-1和流分A-2。
4.将流分A-2减压浓缩干燥,取4.5g于体积百分数为55%至60%的甲醇水溶液溶解,经200g Sephadex LH-20柱色谱分离,以体积百分数为55%至60%的甲醇水溶液为流动相,取得流分A-2-1;
5.将流分A-2-1减压浓缩干燥后,取31mg,经ODS柱色谱分离,以体积百分数为40%至65%的甲醇水溶液为流动相,取得流分A-2-1-1和流分A-2-1-2;
6.对化合物3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯进行鉴定:
流分A-2-1-1经鉴定为化合物3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯,为白色无定形粉末(甲醇)。三氯化铁-铁氰化钾反应呈阳性,Molisch反应阳性,酸水解检出葡萄糖。HR-ESI-MS m/z:533.1429([M+Na]+,C27H26O10Na,Calcd 533.1418)。UV(MeOH)λmax nm(logε)203(4.53),210(4.57),312(1.26)。IR(KBr)vmax 3382,2919,1710,1603,1498,1452,1383.8,1278,1211,1070,1027,967,908,810,783,714,624,588,463cm-1。并利用一维和二维NMR、质谱等技术鉴定其结构。
氢谱和碳谱数据如下:
1H-NMR(600MHz,DMSO-d6),δ:7.94(2H,m,H-2”',6”'),7.68(1H,m,H-4”'),7.53(2H,m,H-3”',5”'),7.45(2H,m,H-2',6'),7.38(2H,m,H-3',5'),7.33(1H,m,H-4'),7.10(1H,d,J=8.8Hz,H-5),7.02(1H,d,J=3.2Hz,H-2),6.75(1H,dd,J=3.2,8.8Hz,H-6),5.24(1H,d,J=12.7Hz,H-7'a),5.22(1H,d,J=12.7Hz,H-7'b),4.82(1H,d,J=7.4Hz,H-1”),4.57(1H,dd,J=2.2,11.9Hz,H-6”a),4.26(1H,dd,J=7.1,11.9Hz,H-6”b),3.70(1H,m,H-5”),3.31(2H,overlap,H-2”,3”),3.28(1H,m,H-4”)。13C-NMR(150MHz,DMSO-d6),δ:165.6(C-7),165.5(C-7”'),152.0(C-3),148.7(C-4),136.1(C-1'),133.3(C-4”'),129.6(C-1”'),129.1(C-2”',6”'),128.6(C-3”',5”'),128.3(C-3',5'),127.9(C-2',4',6'),122.4(C-1),119.8(C-6),118.9(C-5),116.0(C-2),102.0(C-1”),76.3(C-3”),73.7(C-5”),73.3(C-2”),70.0(C-4”),66.1(C-7'),64.1(C-6”)。
从图1A可见:化合物3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的[M+Na]+(C27H26O10Na)的分子量为533.1429。
从图2A可见:特征区内v C=C 1603cm-1及指纹区γ=CH 714cm-1为取代苯的特征吸收峰;v C=O 1710cm-1、v as C―O―C 1278cm-1、v s C―O―C 1027cm-1为酯的一组相关峰;v OH3382cm-1、v=C―O 1211cm-1及v C―O 1070cm-1表明化合物中存在酚和醇结构。
从图3A可见:在312nm处吸收,表明该化合物含有苯结构,且存在与苯环共轭的不饱和基团。
从图4A可见:δ:116.0(C-2)与7.02(1H,d,J=3.2Hz,H-2),118.9(C-5)与7.10(1H,d,J=8.8Hz,H-5),119.8(C-6)与6.75(1H,dd,J=8.8,3.2Hz,H-6),127.9(C-2')与7.45(1H,m,H-2'),128.3(C-3')与7.38(1H,m,H-3'),127.9(C-4')与7.33(1H,m,H-4'),128.3(C-5')与7.38(1H,m,H-5'),127.9(C-6')与7.45(1H,m,H-6'),66.1(C-7')与5.24(1H,d,J=12.7Hz,H-7'a)5.22(1H,d,J=12.7Hz,H-7'b),102.0(C-1”)与4.82(1H,d,J=7.4Hz,H-1”),73.3(C-2”)与3.31(1H,m,H-2”),76.3(C-3”)与3.31(1H,m,H-3”),70.0(C-4”)与3.28(1H,m,H-4”),73.7(C-5”)与3.70(1H,m,H-5”),64.1(C-6”)与4.57(1H,dd,J=11.9,2.2Hz,H-6”a)4.26(1H,dd,J=11.9,7.1Hz,H-6”b),129.1(C-2”')与7.94(1H,m,H-2”'),128.6(C-3”')与7.53(1H,m,H-3”'),133.3(C-4”')与7.68(1H,m,H-4”'),128.6(C-5”')与7.53(1H,m,H-5”'),129.1(C-6”')与7.94(1H,m,H-6”')分别相互关联,其结果与化合物3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的结构相一致。
从图5A可见:δ:127.9(C-2',C-6')与5.24(H-7')和5.22(H-7'),165.5(C-7”')与7.49(H-2”',6”'),165.6(C-7)与5.24(H-7')和5.22(H-7'),148.7(C-4)与4.82(H-1”),165.5(C-7”')与4.57(H-6”)和4.26(H-6”)分别相互关联,其结果与化合物3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的结构相一致。
通过以上鉴定,确定流分A-2-1-1为单体化合物,3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯。
7.对化合物4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯进行鉴定:
流分A-2-1-2经鉴定为化合物4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯,为白色无定形粉末(甲醇)。三氯化铁-铁氰化钾反应呈阳性,Molisch反应阳性,酸水解检出葡萄糖。HR-ESI-MS m/z:559.1582([M+Na]+,C29H28O10Na,Calcd 559.1575)。UV(MeOH)λmax nm(logε)210(4.61),243(1.57),278(3.15)。IR(KBr)vmax 3422,2945,1688,1636,1488,1451,1385,1330,1284,1207,1076,1029,830,787,770,697,554cm-1。并利用一维和二维NMR、质谱等技术鉴定其结构。
氢谱和碳谱数据如下:
1H-NMR(600MHz,DMSO-d6),δ:7.69(2H,m,H-2”',6”'),7.61(1H,d,J=16.0Hz,H-7”'),7.45(3H,overlap,H-2',6',4”'),7.43(3H,overlap,H-2,3”',5”'),7.39(2H,m,H-3',5'),7.35(1H,m,H-4'),7.26(1H,dd,J=3.1,9.1Hz,H-6),6.88(1H,d,J=9.1Hz,H-5),6.62(1H,d,J=16.0Hz,H-8”'),5.32(1H,s,H-7'),4.79(1H,d,J=7.7Hz,H-1”),4.39(1H,dd,J=2.0,11.9Hz,H-6”a),4.21(1H,dd,J=6.6,11.9Hz,H-6”b)。13C-NMR(150MHz,DMSO-d6),δ:167.9(C-7),166.1(C-9”'),155.2(C-4),149.6(C-3),144.6(C-7”'),135.6(C-1'),134.0(C-1”'),130.5(C-4”'),129.0(C-3”',5”'),128.5(C-3',5'),128.4(C-2”',6”'),128.3(C-4'),127.9(C-2',6'),125.1(C-6),118.2(C-5),117.9(C-8”'),117.2(C-2),113.1(C-1),101.6(C-1”),76.1(C-3”),73.7(C-5”),73.1(C-2”),69.8(C-4”),66.6(C-7'),63.5(C-6”)。
从图1B可见:化合物4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的[M+Na]+(C29H28O10Na)的分子量为559.1582。
从图2B可见:特征区内v C=C 1636cm-1表明有双键存在;v C=O 1688cm-1、v as C―O―C1284cm-1、v s C―O―C 1029cm-1为酯的一组相关峰;v OH 3422cm-1、v=C―O 1207cm-1及v C―O1076cm-1表明化合物中存在酚、醇结构。
从图3B可见:在243nm、278nm处吸收,表明该化合物为芳香族化合物,且结构中存在含杂原子的不饱和基团。
从图4B可见:δ:117.2(C-2)与7.43(1H,overlap,H-2),118.2(C-5)与6.88(1H,d,J=9.1Hz,H-5),125.1(C-6)与7.26(1H,dd,J=3.1,9.1Hz,H-6),127.9(C-2')与7.45(1H,m,H-2'),128.5(C-3')与7.39(1H,m,H-3'),128.3(C-4')与7.35(1H,m,H-4'),128.5(C-5')与7.39(1H,m,H-5'),127.9(C-6')与7.45(1H,m,H-6'),66.61(C-7')与5.32(2H,s,H-7'),101.6(C-1”)与4.79(1H,d,J=7.7Hz,H-1”),73.1(C-2”)与3.24(1H,m,H-2”),76.1(C-3”)与3.30(1H,m,H-3”),69.8(C-4”)与3.24(1H,m,H-4”),73.7(C-5”)与3.62(1H,m,H-5”),63.5(C-6”)与4.39(1H,dd,J=2.0,11.9Hz,H-6”a)4.21(1H,dd,J=6.6,11.9Hz,H-6”b),128.4(C-2”')与7.69(1H,m,H-2”'),129.0(C-3”')与7.43(1H,m,H-3”'),130.5(C-4”')与7.45(1H,m,H-4”'),129.0(C-5”')与7.43(1H,m,H-5”'),128.4(C-6”')与7.69(1H,m,H-6”'),144.6(C-6”')与7.61(1H,d,J=16.0Hz,H-7”'),117.9(C-7”)与6.62(1H,d,J=16.0Hz,H-8”')分别相互关联,其结果与化合物4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的结构相一致。
从图5B可见:δ:149.6(C-3)与4.79(H-1”)和6.88(H-5),155.2(C-4)与7.43(H-2)和7.26(H-6),167.9(C-7)与5.32(H-7'),66.6(C-7')与7.45(H-2',6'),134.0(C-1”')与6.62(H-8”'),128.4(C-2”',6”')与7.61(H-7”'),166.1(C-9”')与4.39(H-6”a),4.21(H-6”b)和7.61(H-7”')分别相互关联,其结果与化合物4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯的结构相一致。
通过以上鉴定,说明流分A-2-1-2为单体化合物,4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯。
四、本发明琼花提取物和活性化合物的抗炎活性考察
本发明申请以抑制小鼠单核巨噬细胞NO生成率作为抗炎活性的检测指标。以LPS刺激小鼠单核巨噬细胞,使iNOS高表达,产生大量的NO,NO在液体培养基中迅速转变为亚硝酸盐,与Griess试剂反应后溶液呈红色,在540nm处有吸收。通过计算反应的亚硝酸盐的量来测定溶液中NO的量,进而得出药物对NO释放的影响。
首先取活力良好的RAW264.7细胞,将细胞浓度调节至5×105/ml,接种到96孔板上,每孔接种100μl,置于37℃、5%CO2培养箱中培养;用DMSO溶解供试样品,然后用培养液进行梯度稀释;每孔加入LPS(终浓度1μg/ml)和不同浓度的样品溶液,共100μl,置于37℃、5%CO2培养箱中培养24h;实验中设空白调零组、正常组(不加LPS、不加样品)、LPS模型组(不加样品)及阳性对照组,每个样品测定均平行重复三次;每孔取50μl培养液上清至另一96孔板中,室温下加入试剂盒中的Griess试剂I和Griess试剂II各50μl;室温下反应10min,在波长540nm处测定其OD值。绘制NaNO2标准曲线,根据标准曲线计算化合物对NO释放的抑制率。
琼花乙酸乙酯层两种新化合物对NO的抑制作用
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,作出的若干改进和润饰也应视为本发明的保护范围。
Claims (6)
2.权利要求1所述抗炎活性成分的提取分离方法,其特征在于,包括以下步骤:
(1)对所述琼花提取物进行浓缩干燥,取得浸膏,将浸膏溶解于蒸馏水中,采用乙酸乙酯进行萃取,取得乙酸乙酯萃取液,此萃取液进行减压浓缩后,获得乙酸乙酯萃取浸膏;
(2)乙酸乙酯萃取浸膏上样于MCI微孔树脂色谱柱,以体积百分数为80%至90%的甲醇水溶液为流动相,进行洗脱,收集此流动相的洗脱物,减压浓缩得到流分A;
(3)将流分A上样于硅胶柱色谱,先后以体积比为100:4和100:8的氯仿和甲醇混合液为流动相,进行洗脱,分别收集洗脱物,得到两个流分,流分A-1和流分A-2;
(4)流分A-2经Sephadex LH-20柱色谱进行分离,以体积百分数为55%至60%的甲醇水溶液为流动相,经Sephadex LH-20柱色谱进行梯度洗脱,收集此流动相的洗脱物,减压浓缩得流分A-2-1;
(5)流分A-2-1经ODS柱色谱进行分离,以体积百分数为40%至65%的甲醇水溶液为流动相进行梯度洗脱,收集此流动相的洗脱物,减压浓缩取得流分A-2-1-1和流分A-2-1-2;
流分A-2-1-1经鉴定,即为所述化合物1:3-羟基-4-(6-苯甲酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯;
流分A-2-1-2经鉴定,即为所述化合物2:4-羟基-3-(6-肉桂酰基-β-D-吡喃葡萄糖基)苯甲酸苯甲酯。
3.根据权利要求2所述的提取分离方法,其特征在于,所述步骤(1)中浓缩干燥的温度为40℃。
4.根据权利要求2所述的提取分离方法,其特征在于,步骤(2)中所述的乙酸乙酯萃取浸膏先用体积百分数为80%至90%的甲醇水溶液溶解,然后再上样。
5.一种组合物,其特征在于,该组合物包含权利要求1所述抗炎活性成分,以及药学可接受的载体或赋形剂。
6.权利要求1所述抗炎活性成分在制备抗炎药物中的应用。
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