CN1903241B - 一种三七药材的提取分离方法 - Google Patents
一种三七药材的提取分离方法 Download PDFInfo
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Abstract
本发明公开了三七标准化提取分离方法，采用该方法可较大程度地将中药材中化学成分提取出来并进一步分离获得三七中不同极性的化学组分；具体的说就是将三七药材按极性分成若干化学组分，每个组分中仅包含几个主要化合物，由这些药材组分构成一个药材组分库。对药材组分库能够进行药物筛选，从而发现新药。该标准化提取分离方法不需要对每个药材都建立一套提取分离方法，大大缩短了药材提取分离的周期，同时也减少人力物力的消耗；该方法简便、推广性好，适用大部分药材。
Description
技术领域
本发明属于医药领域，具体而言是涉及三七提取、分离标准化。
背景技术
目前，在全球范围内，中草药都有一定的市场，随着人们对健康要求认识水平的增高以及人口的老龄化，亚健康状态化，人们更加渴望回归自然，利用纯天然程度高的药物治疗、预防一些化学合成药物所不能解决得问题，因此天然植物药的应用超出它原来民族传统文化的背景。从天然药物中寻求副作用小、且物美价廉的药物成为世界各国医药企业所追逐的目标。欧共体对草药进行了统一立法，加拿大和澳大利亚等国草药地位已经合法化，美国政府也已起草了植物药管理办法，开始接受天然药物的复方混合制剂作为治疗药，这些为中药作为治疗药进入国际医药市场提供了良好的国际环境。另一方面，随着全球经济一体化进程的加快，特别是我国正式加入WTO，中国医药市场融入国际医药大市场的广度和深度将进一步加剧。面临强大跨国医药集团的激烈竞争以及日本、韩国、印度、泰国等亚洲国家传统医药产品和德国、法国等欧洲国家植物药的巨大冲击，我国传统中药产生的众多产品由于尚不能符合国际医药市场的标准和要求而被拒之门外。
中药材提取的标准化和中药制备方法的标准化是中成药走向国际市场或者真正实现大工业生产的关键环节，也是中国医药工作者和国外研究天然植物药的科研人员一直努力研究的方向。目前关于中药的提取方法是中药领域研究的重点，科研人员一直将研究的目光着重于采用何种方法才能从中药材中获得的更多的有效成分，因此目前的中药材提取的局面是：针对不同的中药材其有效成分的提取方法也不同，而针对不同的中药材采用不同的提取方法需要有大量不同的提取设备用于支持中药材的提取，这不适于中药材提取的标准化。
三七为五加科植物三七Panax notoginseng(Burk.)F.H.Chen的干燥根。中医认为，其味甘、微苦，性温，归肝、胃经。具有散瘀止血，消肿定痛之功效，适用于治疗咯血，吐血，衄血，便血，崩漏，外伤出血，胸腹剌痛，跌扑肿痛等。现代研究表明，三七中主要含人参皂甙(Ginsenosides)Rb1、Rd、Re、Rg1、Rg2、Rh，20-O-葡萄糖人参皂甙Rf，三七皂甙(Notoginsenoside)R1、R2、R3、R4，七叶胆皂甙(Gypeno-side)X VII，尚含人参皂甙Rb2。还含挥发油，有α-及β-愈创烯(α-，β-guaiene)，另外有α-古巴烯(α-copaene)、δ-愈创烯、花柏烯(cuparene)、α-，β-，γ-榄香烯(α-，β-，γ-elemene)、α-依兰油烯(α-muurolene)、α-古芸烯(α-gurjunene)、十六酸甲酯、十六酸乙酯、十七碳二烯酸甲酯、十八碳二烯酸乙酯、邻苯二甲酸二叔丁酯(benzene-diformic acid ditert-butylate)、十八碳二烯酸、异丙苯、环十二碳酮(cy-clodode-canone)、1-甲基-4-过氧甲硫基[2，2，2]辛烷、十四烷、十六烷、十七烷、十八烷、十九烷、廿烷、廿一烷、廿二烷。水提取液中含一种具止血活性的三七素(N-oxalo-L-α，β-diaminopro-pionic acid)。另含槲皮素、三七黄酮B、β-谷甾醇、β-谷甾醇-D-葡萄糖甙、蔗糖。
如何确定一种提取、分离标准化方法，使三七中的药物活性成分不仅能够提取完全，还可以通过分离方法进一步分离所获得的药物活性成分。该提取、分离标准化的确立是目前中药实现现代化的关键因素。
发明内容
本发明的目的在于提供一种三七提取、分离标准化。具体的说就是将三七提取物分成若干组分，每个组分包含几个主要化合物，由这些药材组分构成了一个药材组分库。对药材组分库能够进行药物筛选，从而发现新药。
为了实现三七提取的现代化、标准化，本发明人通过大量的试验，对目前三七的有效成分的提取方法进行归纳和整理，以寻求一种可标准化的提取方法，即在该提取条件下采用该标准提取方法对三七进行提取，可以最大限度的获得中药中的有效成分。
本发明所采用的三七提取、分离标准化是本发明人通过试验，对同一味中药材采用不同的提取方法进行比较后，所得到的可适于工业化生产的三七提取、分离标准化。
本发明可以通过下列步骤实施：
(1)提取工艺：称取三七药材，将其粉碎后过筛，然后加入乙酸乙酯和乙醇，加热提取得提取液fr.1；在药渣中加入乙醇，加热提取得提取液fr.2；在药渣中最后加入水，加热提取得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩成浸膏后，用硅胶拌样，采用正相硅胶柱对其进行分离，首先用石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换氯仿和甲醇作为流动相，得洗脱液fr.5，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩成浸膏后，用甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用低浓度的甲醇作为流动相，得洗脱液fr.7，然后改换中等浓度的甲醇作为流动相，得洗脱液fr.8，最后用纯甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱分离fr.8；色谱柱为半制备柱，流动相为水和乙腈，梯度洗脱，在相应的时间段收集馏分，获得经过了进一步分离的各个组分。
优选的本发明可以通过下列步骤实施：
(1)提取工艺：称取三七药材，将其粉碎后过筛，然后加入5～12倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.1；在药渣中加入5～12倍量70％乙醇，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.2；在药渣中最后加入水，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩成浸膏后，用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩成浸膏后，用2～10％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用2～10％甲醇作为流动相，得洗脱液fr.7，然后改换40～80％甲醇作为流动相，得洗脱液fr.8，最后用100％甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱离fr.8；色谱柱为半制备柱(Lichrospher C18；10.0mm×250mm，5μm)，流动相为水和乙腈，梯度洗脱，流速为3ml/min，柱温为室温，在相应的时间段收集馏分，获得经过进一步分离的各个组分。
最佳的本发明可以通过下列步骤实施：
(1)提取工艺：称取三七药材，将其粉碎后过筛，然后加入8倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.1；在药渣中加入8倍量70％乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.2；在药渣中最后加入水，加热回流1小时，提取2次，合并滤液得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩成浸膏，用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩成浸膏，用5％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用5％甲醇作为流动相，得洗脱液fr.7，然后改换60％甲醇作为流动相，得洗脱液fr.8，最后用100％甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱分离fr.8；
fr.8分离条件：色谱柱为Agilent制备柱(Zorbax SB-C18；21.2mm×250mm)；采用梯度洗脱，流动相为水(A)和乙腈(B)，流速为10ml/min，柱温为室温，洗脱梯度如下：
0min时，流动相A为90％的水，流动相B为10％的乙腈溶液；
15min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
20min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
35min时，流动相A为58％的水，流动相B为42％的乙腈溶液；
45min时，流动相A为5％的水，流动相B为95％的乙腈溶液；
fr.8分离结果：由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min；
组分fr.82，收集时间7.4-13.4min；
组分fr.83，收集时间13.4-17.8min；
组分fr.84，收集时间17.8-20.9min；
组分fr.85，收集时间20.9-27.7min；
组分fr.86，收集时间27.7-34.3min；
组分fr.87，收集时间34.3-41.1min；
组分fr.88，收集时间41.1-45.0min。
为了获得具体的三七有效成分，最佳的本发明提取分离方法为：
(1)提取工艺：称取三七药材250g，将其粉碎后过筛，然后加入8倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.1。在药渣中加入8倍量70％乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.2。在药渣中最后加入水，加热回流1小时，提取2次，合并滤液得提取液fr.3。
(2)分离工艺：将提取液fr.1浓缩得3.9g浸膏，取fr.1浸膏3.1g用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，浓缩得26.7mg样品，最后用甲醇作为流动相，得洗脱液fr.6。将提取液fr.2浓缩得23.6g浸膏，取20.0g浸膏用5％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用5％甲醇作为流动相，得洗脱液fr.7，然后改换60％甲醇作为流动相，得洗脱液fr.8，浓缩得3.2g样品，最后用100％甲醇溶液作为流动相，得洗脱液fr.9。
(3)制备分离工艺：本发明中为了从步骤(2)中获得三七提取物中fr.8更加具体的有效成分，用制备液相色谱继续分离fr.8。
fr.8分离条件：色谱柱为Agilent制备柱(Zorbax SB-C18；21.2mm×250mm)；采用梯度洗脱，流动相为水(A)和乙腈(B)，流速为10ml/min，柱温为室温，洗脱梯度如下：
0min时，流动相A为90％的水，流动相B为10％的乙腈溶液；
15min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
20min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
35min时，流动相A为58％的水，流动相B为42％的乙腈溶液；
45min时，流动相A为5％的水，流动相B为95％的乙腈溶液；
fr.8分离结果：取fr.81.8g，用20％甲醇水溶液溶解，由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min，65.3mg；
组分fr.82，收集时间7.4-13.4min，116.6mg；
组分fr.83，收集时间13.4-17.8min，94.7mg；
组分fr.84，收集时间17.8-20.9min，151.8mg；
组分fr.85，收集时间20.9-27.7min，462.6mg；
组分fr.86，收集时间27.7-34.3min，142.4mg；
组分fr.87，收集时间34.3-41.1min，408.8mg；
组分fr.88，收集时间41.1-45.0min，68.7mg。
本发明中，三七各组分中所含化合物见表1，其分析鉴定方法参见实施例三。
表1.三七各组分中所含化合物
以上三七及其提取溶液在工业化提取时可按照相应的比例增大或减少，如大规模生产可以以公斤或以吨为单位，小规模生产也可以以克为单位，重量可以增大或减小，但其重量配比比例不变。
本发明所建立的提取、分离标准化可以适用于目前中药中的任何一种中药材，例如可用于阿魏、艾叶、安息香、柏子仁、鳖甲、槟榔、薄荷、蓖麻子、蓄、补骨脂、板蓝根、荜茇、巴豆、巴戟天、北豆根、北沙参、白及、白头翁、白芍、白芷、白附子、白茅根、白果、白前、白扁豆、自蔹、白鲜皮、白薇、半边莲、半枝莲、半夏、百合、冰片、柴胡、蝉蜕、楮实子、常山、椿皮、穿山甲、穿心莲、赤小豆、赤石脂、赤芍、苍术、苍耳子、沉香、垂盆草、侧柏叶、草乌、草乌叶、草豆蔻、草果、川贝母、川牛膝、川乌、川芎、川楝子、车前子、淡豆豉、党参、淡竹叶、杜仲、独活、胆南星、大蓟、大腹皮、牡丹皮、煅石膏、冬瓜皮、冬虫夏草、地龙、地肤子、地骨皮、熟地黄、地锦草、地榆、当归、灯心草、丁香、刀豆、大青叶、大枣、大黄、鹅不食草、莪术、儿茶、榧子、浮萍、萆解、覆盆子、佛手、附子、茯苓、防己、防风、番泻叶、蜂蜜、蛤蚧、桂枝、葛根、藁本、高良姜、骨碎补、谷芽、谷精草、狗脊、枸杞子、枸骨叶、钩藤、甘松、甘草、甘遂、瓜蒌、瓜蒌子、瓜蒌皮、关木通、干姜、炮姜、干漆、鹤虱、黄芪、黄精、海藻、槐花、海风藤、荷叶、黄芩、黄连、黄柏、花椒、何首乌、虎杖、胡黄连、厚朴、化橘红、火麻仁、合欢皮、合欢花、红大戟、红花、黑芝麻、菊花、僵蚕、桔梗、橘核、姜黄、鸡血藤、鸡冠花、金果榄、金沸草、金荞麦、金钱草、金银花、降香、荆芥、韭菜子、决明子、款冬花、诃子、苦杏仁、苦参、苦楝皮、莱菔子、雷丸、凌霄花、鹿衔草、漏芦、路路通、莲子、络石藤、芦荟、芦根、两头尖、两面针、连翘、灵芝、罗布麻叶、罗汉果、荔枝核、龙胆、龙眼肉、老鹳草、墨旱莲、麻黄、蔓荆子、满山红、满山红油、密蒙花、梅花、麻黄、麦冬、麦芽、玫瑰花、明党参、马鞭草、马兜铃、马钱子、马钱子粉、马勃、马齿苋、木瓜、木香、木贼、南沙参、女贞子、牛蒡子、牛膝、藕节、蒲黄、蒲公英、枇杷叶、佩兰、片姜黄、瞿麦、秦皮、拳参、芡实、羌活、青木香、青风藤、青皮、青葙子、青蒿、青黛、茜草、牵牛子、前胡、千年健、千金子、秦艽、蕤仁、肉豆蔻、肉苁蓉、肉桂、人参、人参叶、石菖蒲、锁阳、桑叶、商陆、桑椹、蛇床子、桑白皮、桑枝、桑枝、桑寄生、娑罗子、酸枣仁、射干、苏合香、沙苑子、使君子、柿蒂、砂仁、山豆根、山茱萸、山药、山慈菇、山楂、小蓟、升麻、水牛角、水牛角浓缩粉、石韦、石决明、石斛、石榴皮、生姜、丝瓜络、三七、三棱、葶苈子、菟丝子、桃仁、通草、檀香、天花粉、天竺黄、天南星、天麻、天葵子、太子参、土荆皮、土茯苓、吴茱萸、威灵仙、王不留行、五加皮、五味子、五倍子、瓦楞子、乌药、乌梅、夏天无、续断、旋覆花、豨莶草、薤白、夏枯草、辛夷、香加皮、香附、香橼、香薷、小茴香、仙茅、仙鹤草、玄参、玄明粉、西洋参、血余炭、血竭、徐长卿、淫羊藿、益母草、银杏叶、薏苡仁、银柴胡、远志、芫花、郁李仁、郁金、鱼腥草、茵陈、鸦胆子、月季花、玉竹、延胡索、浙贝母、猪牙皂、紫苏子、紫菀、紫花地丁、紫草、猪苓、皂角刺、知母、泽兰、泽泻、珍珠母、枳实、栀子。
按照本发明方法所获得的三七有效成分可以制成药剂学上任何一种形式，包括针剂和口服制剂。其中针剂包括注射液、滴注液、粉针剂；口服制剂包括颗粒剂、片剂、冲剂、散剂、口服液、糖衣片剂、薄膜衣片剂、肠溶衣片剂、胶囊剂、硬胶囊剂、软胶囊剂、口含剂、颗粒剂、丸剂、膏剂、丹剂、喷雾剂、滴丸剂、崩解剂、口崩片、微丸等。
对于本领域技术人员而言，根据本发明所公开的技术内容，本领域技术人员将很清楚本发明的其它实施方案，本发明实施例仅作为示例。在不违反本发明主旨及范围的情况下，可对本发明进行各种改变和改进，例如所选用的溶液可以是其他低级醇或者是其他有机溶剂，但只要使用本发明所述的提取方法，均在本发明保护范围之内。
附图说明
下面给出三七指纹图谱，三七水溶性各组分紫外光谱图、三七水溶性各组分质谱图，旨在进一步说明本发明，但对本发明并不构成限制。
图1三七指纹图谱
图2三七水溶性各组分紫外图谱
图3三七水溶性各组分质谱图
具体实施方式
实施例一
(1)提取工艺：称取250g三七药材，将其粉碎后过筛，然后加入乙酸乙酯和乙醇，加热提取得提取液fr.1；在药渣中加入乙醇，加热提取得提取液fr.2；在药渣中最后加入水，加热提取得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩得3.6g浸膏，取fr.1浸膏3g用硅胶拌样，采用正相硅胶柱对其进行分离，首先用石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换氯仿和甲醇作为流动相，得洗脱液fr.5，浓缩得25.1mg样品，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩得21.8g浸膏，取20.0g浸膏甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用低浓度的甲醇作为流动相，得洗脱液fr.7，然后改换中等浓度的甲醇作为流动相，得洗脱液fr.8，浓缩得2.86g样品，最后用纯甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱分离fr.8；色谱柱为半制备柱，流动相为水和乙腈，梯度洗脱，在相应的时间段收集馏分，获得经过了进一步分离的各个组分。
fr.8分离结果：取fr.82.0g，用20％甲醇水溶液溶解，由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min，64.3mg；
组分fr.82，收集时间7.4-13.4min，113.3mg；
组分fr.83，收集时间13.4-17.8min，95.9mg；
组分fr.84，收集时间17.8-20.9min，148.5mg；
组分fr.85，收集时间20.9-27.7min，459.3mg；
组分fr.86，收集时间27.7-34.3min，138.9mg；
组分fr.87，收集时间34.3-41.1min，401.4mg；
组分fr.88，收集时间41.1-45.0min，65.5mg。
实施例二
(1)提取工艺：称取500g三七药材，将其粉碎后过筛，然后加入5～12倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.1；在药渣中加入5～12倍量70％乙醇，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.2；在药渣中最后加入水，加热回流0.5～3小时，提取1～3次，合并滤液得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩得7.2g浸膏，取fr.1浸膏6g用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，浓缩得50.5mg样品，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩得44.4g浸膏，取40.0g浸膏2～10％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用2～10％甲醇作为流动相，得洗脱液fr.7，然后改换40～80％甲醇作为流动相，得洗脱液fr.8，浓缩得6.12g样品，最后用100％甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱离fr.8；色谱柱为半制备柱(Lichrospher C18；10.0mm×250mm，5μm)，流动相为水和乙腈，梯度洗脱，流速为3ml/min，柱温为室温，在相应的时间段收集馏分，获得经过进一步分离的各个组分。
fr.8分离结果：取fr.83.5g，用20％甲醇水溶液溶解，由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min，128.2mg；
组分fr.82，收集时间7.4-13.4min，226.7mg；
组分fr.83，收集时间13.4-17.8min，180.3mg
组分fr.84，收集时间17.8-20.9min，244.8mg；
组分fr.85，收集时间20.9-27.7min，908.6mg；
组分fr.86，收集时间27.7-34.3min，269.4mg；
组分fr.87，收集时间34.3-41.1min，801.1mg；
组分fr.88，收集时间41.1-45.0min，128.2mg。
实施例三
一、三七药材的提取分离
(1)提取工艺：称取三七药材250g，将其粉碎后过筛，然后加入8倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.1。在药渣中加入8倍量70％乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.2。在药渣中最后加入水，加热回流1小时，提取2次，合并滤液得提取液fr.3。
(2)分离工艺：将提取液fr.1浓缩得3.9g浸膏，取fr.1浸膏3.1g用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，浓缩得26.7mg样品，最后用甲醇作为流动相，得洗脱液fr.6。将提取液fr.2浓缩得23.6g浸膏，取20.0g浸膏用5％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用5％甲醇作为流动相，得洗脱液fr.7，然后改换60％甲醇作为流动相，得洗脱液fr.8，浓缩得3.2g样品，最后用100％甲醇溶液作为流动相，得洗脱液fr.9。
(3)制备分离工艺：本发明中为了从步骤(2)中获得三七提取物中fr.8更加具体的有效成分，用制备液相色谱继续分离fr.8。
fr.8分离条件：色谱柱为Agilent制备柱(Zorbax SB-C18；21.2mm×250mm)；采用梯度洗脱，流动相为水(A)和乙腈(B)，流速为10ml/min，柱温为室温，洗脱梯度如下：
0min时，流动相A为90％的水，流动相B为10％的乙腈溶液；
15min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
20min时，流动相A为72％的水，流动相B为28％的乙腈溶液；
35min时，流动相A为58％的水，流动相B为42％的乙腈溶液；
45min时，流动相A为5％的水，流动相B为95％的乙腈溶液；
fr.8分离结果：取fr.81.8g，用20％甲醇水溶液溶解，由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min，65.3mg；
组分fr.82，收集时间7.4-13.4min，116.6mg；
组分fr.83，收集时间13.4-17.8min，94.7mg；
组分fr.84，收集时间17.8-20.9min，151.8mg；
组分fr.85，收集时间20.9-27.7min，462.6mg；
组分fr.86，收集时间27.7-34.3min，142.4mg；
组分fr.87，收集时间34.3-41.1min，408.8mg；
组分fr.88，收集时间41.1-45.0min，68.7mg。
二、分析
2.1试剂与仪器
Agilent 1100高效液相色谱-质谱联用仪(美国安捷伦公司)，配在线真空脱气机、四元低压泵、自动进样器、柱温箱、DAD检测器、1946D电喷雾四级杆质谱检测器、Chemstation色谱工作站；R-200型旋转蒸发仪(瑞士BUCHI公司)；飞鸽牌TGL-16G高速台式离心机(上海安亭科学仪器厂)；METTLER-AE240型电子天平(梅特勒-托利多仪器有限公司)。
乙腈为色谱纯试剂(MERCK)，水为娃哈哈纯净水(杭州娃哈哈集团)，乙酸为分析纯(杭州试剂厂)。
2.2分析方法
样品来源：三七组分fr.81 1.11mg、fr.82 1.20mg、fr.83 1.16mg、fr.84 1.12mg、fr.851.11mg、fr.86 1.11mg、fr.87 1.21mg、fr.88 1.18mg。
样品制备：样品用1ml 50％甲醇水溶解，超声，离心(10000r/min)，备用。
色谱条件：色谱柱Agilent Zorbax SB-C18柱(4.6mm×150mm，5μm)；采用梯度洗脱，流动相A相为0.01％冰醋酸水溶液，流动相B相为含0.01％冰醋酸的乙腈溶液；梯度洗脱程序如下：0分钟时，流动相A为95％的0.01％冰醋酸水溶液、流动相B为5％的0.01％冰醋酸乙腈溶液；10分钟时，流动相A为70％的0.01％冰醋酸水溶液、流动相B为30％的0.01％冰醋酸乙腈溶液；30分钟时，流动相A为50％的0.01％冰醋酸水溶液、流动相B为50％的0.01％冰醋酸乙腈溶液；流速0.5mL/min；柱温30℃；DAD检测在190-400nm范围内扫描；进样量5μL。
质谱条件：正负离子扫描模式，扫描范围100-2000；干燥气(N2气)流速10L/min，雾化温度350℃，毛细管电压3500V，裂解电压100V。
ELSD条件：氮气1.8L/min，漂移管温度：105℃。
2.3分析结果
分析结果：图2是三七水溶性各组分紫外图谱，图3是三七水溶性各组分质谱图。三七组分中化合物的鉴定结果[1-5]见表2，紫外最大吸收波长都为203nm。
表2.三七组分化合物鉴定结果
参考文献：
1.DNP(天然化合物数据库)。
2.W.G.Ma，M.Mizutani，K.E.Malterud，et al，Saponins from the roots of Panax notoginseng.Phytochemistry 52(1999)，1133-1139。
3.L.Li，R.Tsao，J.P.Dou，et al.Detection of saponins in extract of Panax notoginseng by liquidchromatography-electrospray ionization-mass spectrometry.Analytica Chimica Acta 536(2005)，21-28。
4.S.Y.Liu，M.Cui，Z.Q.Liu，et al.Structural Analysis of Saponins from Medicinal Herbs UsingElectrospray Ionization Tandem Mass Spectrometry.J.Am.Soc.Mass Spectrom 2004(15)，133-141。
5.G.C.Kite，M.J.R.Howes，C.J.Leon，et al.Liquid chromatography/mass spectrometry ofmalonyl-ginsenosides in the authentication of ginseng.Rapid Communications in MassSpectrometry，2003(17)，238-244。
三、三七组分药效筛选实验
3.1药理模型：乳鼠心肌细胞缺血缺氧模型
原代心肌细胞培养 出生1～3天SD乳鼠处死后，取心脏，经PBS液清洗后剪成1mm3左右的碎块。用0.125％胰蛋白酶(Sigma，USA)+0.05％胶原酶II(Gibco，USA)于37℃消化3～4次。差速贴壁法分离成纤维细胞1.5小时后，细胞悬液转移至48孔板中(每孔约4×105细胞)。经DMEM(Gibco，USA)加10％胎牛血清(Falcon，USA)培养3～6天的细胞供药效筛选。筛选前1天替换为无血清培养液。培养3～6天的心肌细胞，PBS洗涤后加入含药培养液。置于95％N2和5％CO2培养箱中缺氧6小时。然后在CO2培养箱中复氧3小时。取细胞上清液测定LDH含量。
给药方案 提取得到的三七提取物用无糖Hanks液配成10-4g/mL供试液，脂溶性成分可加入少量DMSO助溶(DMSO终浓度控制在0.2％以下)。各组分在培养液中的终浓度控制在10-5g/mL。
乳酸脱氢酶含量测定 细胞培养液中乳酸脱氢酶含量能够表示细胞损伤程度。漏入上清液中的乳酸脱氢酶含量越高，表明细胞损伤也显著。乳酸脱氢酶测定试剂盒购自南京建成生物工程研究所。测定方法为：取30μl细胞上清液，加入50μl基质缓冲液及10μl乳酸脱氢酶辅酶，37℃振荡15分钟，再加入50μl 2，4-二硝基苯肼，37℃振荡15分钟。平行空白。取反应液50μl加入200μl 0.4mol/L氢氧化钠溶液，静置3～4分钟后，用酶标仪于450nm测定光度值。
药效结果 所有数据用均值±方差表示。采用单边方差分析和T检验进行统计学分析。与模型组相比，P＜0.05认为显著有效。药效筛选结果见表3。根据心肌细胞乳酸脱氢酶(LDH)筛选结果，三七组分fr.81，fr.84，fr.88对降低LDH释放有非常显著效果，组分fr.87有效果。
表3.心肌细胞筛选结果
3.2脐静脉内皮细胞缺氧复氧模型
原代脐静脉内皮细胞培养 取健康新生儿脐带，用30～50ml Hanks液洗净静脉血管内的残留血迹。视脐带长度加入相应量的0.1％胶原酶I，转入培养箱消化15～20分钟。随后将脐带内消化液小心收集到烧杯中，并用Hanks液将烧杯润洗两次，一并收集到烧杯中分装于离心管，900rpm离心10分钟。吸去上清液，用M199培养液(含10％胎牛血清，100U/ml双抗，0.15mg/ml Heparin，10μM VC)充分溶解沉淀。将所得细胞悬液分装于5cm2培养瓶，置于培养箱内培养。第二天换成采用含30μg/ml ECGS的M199培养液，之后每三天换一次培养液直至细胞铺满底面。所用细胞均为原代内皮细胞。造模前将培养瓶内细胞接种至96孔板并培养一天，所用细胞量为3.5～4万/孔。造模时，吸弃旧的M199培养液，加入含药无酚红M199培养液，每孔总量为100μl。置于95％N2和5％CO2培养箱中缺氧12小时，然后在CO2培养箱中复氧2小时。取细胞上清液测定LDH含量和NO含量。
给药方案 提取得到的三七提取物用无糖Hanks液配成10-4g/mL供试液，脂溶性成分可加入少量DMSO助溶(DMSO终浓度控制在0.2％以下)。各组分在无酚红M199培养液中的终浓度控制在10-5g/mL。
NO含量测定 采用Greiss试剂法测定，取90μl细胞上清液，加入等量Greiss试剂，室温下静置10分钟，用酶标仪于550nm测定吸光度值。
药效结果 所有数据用均值±方差表示。采用单边方差分析和T检验进行统计学分析。与模型组相比，P＜0.05认为显著有效。药效筛选结果见表4。三七7个组分具有抑制内皮细胞缺氧-复氧后NO过度表达的效果，fr.84非常显著有效，fr.81、fr.83、fr.88有效。
表4.内皮细胞筛选结果
以上试验结果说明，采用本发明中药材标准化提取方法获得的中药材有效成分可以用作制备药物。
Claims (1)
1.三七提取、分离标准化方法，包括如下步骤：
(1)提取工艺：称取三七药材，将其粉碎后过筛，然后加入8倍量体积比为1∶1的乙酸乙酯和乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.1；在药渣中加入8倍量70％乙醇，加热回流1小时，提取2次，合并滤液得提取液fr.2；在药渣中最后加入水，加热回流1小时，提取2次，合并滤液得提取液fr.3；
(2)分离工艺：将提取液fr.1浓缩成浸膏，用硅胶拌样，采用正相硅胶柱对其进行分离，首先用体积比为50∶1的石油醚和乙酸乙酯作为流动相，得洗脱液fr.4，然后改换体积比为10∶1的氯仿和甲醇作为流动相，得洗脱液fr.5，最后用甲醇作为流动相，得洗脱液fr.6；将提取液fr.2浓缩成浸膏，用5％甲醇溶解上样，采用ODS-C18柱对其进行分离，首先用5％甲醇作为流动相，得洗脱液fr.7，然后改换60％甲醇作为流动相，得洗脱液fr.8，最后用100％甲醇溶液作为流动相，得洗脱液fr.9；
(3)制备分离工艺：用制备液相色谱分离fr.8；
fr.8分离条件：色谱柱为Agilent制备柱，型号为Zorbax SB-C18；21.2mm×250mm；采用梯度洗脱，流动相A为水，流动相B为乙腈，流速为10ml/min，柱温为室温，洗脱梯度如下：
0min时，流动相A为90％，流动相B为10％；
15min时，流动相A为72％，流动相B为28％；
20min时，流动相A为72％，流动相B为28％；
35min时，流动相A为58％，流动相B为42％；
45min时，流动相A为5％，流动相B为95％；
fr.8分离结果：由制备液相色谱分离得到的组分及相应的收集时间如下：
组分fr.81，收集时间3.0-7.4min；
组分fr.82，收集时间7.4-13.4min；
组分fr.83，收集时间13.4-17.8min；
组分fr.84，收集时间17.8-20.9min；
组分fr.85，收集时间20.9-27.7min；
组分fr.86，收集时间27.7-34.3min；
组分fr.87，收集时间34.3-41.1min；
组分fr.88，收集时间41.1-45.0min。
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