CN116655712A - 一种基于槐米水提液快速制备高纯度芦丁的方法 - Google Patents
一种基于槐米水提液快速制备高纯度芦丁的方法 Download PDFInfo
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Abstract
本发明公开了一种基于槐米水提液快速制备高纯度芦丁的方法,属于中药成分分离制备技术领域。具体为:将槐米水提液在4~30℃下静置12~36h,过滤、干燥获得芦丁粗品析出物,将芦丁粗品析出物用甲醇溶解,注入制备型高效液相色谱仪,选取芦丁段洗脱液,得到芦丁。该方法以槐米为原料建立了芦丁快速、环保、有效降低成本的制备方法,为其提供了有效的资源可持续保障。
Description
技术领域
本发明属于中药成分分离制备技术领域,具体涉及一种基于槐米水提液快速制备高纯度芦丁的方法。
背景技术
槐米为豆科植物槐Sophorajaponica L.的干燥花蕾,夏季花蕾形成时采收,及时干燥,除去枝、梗及杂质。其性苦,微寒。归肝、大肠经。具有凉血止血,清肝泻火的功效。用于便血,痔血,血痢,崩漏,吐血,衄血,肝热目赤,头痛眩晕等病症。槐米主含黄酮类、皂苷类、脂肪酸类、多糖等成分,具有抗炎、抗菌、抗氧化、降血糖、增强免疫力等作用。
槐米所含黄酮类物质以芦丁为主,芦丁又名芸香苷,具有抗氧化、抗炎、改善糖脂代谢、保护心血管等多种药理活性。
芦丁存在于芸香叶、烟叶、橙皮、番茄等内,槐花米和荞麦花内含量尤其丰富,大多学者主要从槐米中提取芦丁,槐米提取芦丁的方法主要有热水提取法、醇提法、超声辅助提取法、微波辅助提取法和碱提酸沉提取法等,其中广泛使用的为碱提酸沉提取法,具体操作是槐米经洗涤后,用热水和石灰乳(调pH至7.5-8)煮沸20min,添加硼砂,在95-100℃保温半小时,趁热过滤,用盐酸将滤液调至pH=6-7,冷却至30℃以下,静置析出结晶,分离,得芦丁粗品,经溶解、再结晶、干燥即得成品,上述方法具有耗时较长、操作繁琐,有机试剂用量大的缺点,所得成品中含有一些与芦丁结构非常接近的杂质,因此探寻一种方法相对简单,提取率、所得产品纯度相对较高的芦丁制备方法具有极为重要的意义。
发明内容
针对现有技术中从槐米中提取芦丁的方法耗时长、有机试剂使用量大且纯度相对较低的问题,本发明提供了一种基于槐米水提液快速制备高纯度芦丁的方法,该方法操作简单,可从槐米中快速提取分离出芦丁,为芦丁的制备研究提供了技术支持。
本发明通过以下技术方案实现:
一种基于槐米水提液快速制备高纯度芦丁的方法,将槐米水提液在4~30℃下静置12~36h,过滤、干燥获得芦丁粗品析出物,利用制备型高效液相技术分离得到芦丁;
制备型高效液相技术具体为:将芦丁粗品析出物用甲醇溶解,注入制备型高效液相色谱仪,选取芦丁段洗脱液,得到芦丁;所述的高效液相色谱条件为色谱柱:Zafex JX-C18,250 ×4.6mm,5µm;流动相:甲醇-0.4%磷酸水梯度洗脱,进样量5µL,流速1ml/min,柱温30℃,检测波长360nm。
进一步地,所述的槐米水提液的制备方法为:取适量槐米粗粉,加入一定10~20倍质量的水加热回流0.5~1.5h,过滤,获得槐米水提液。
进一步地,所述的甲醇-0.4%磷酸水梯度洗脱程序为:
。
进一步地,所述的芦丁段洗脱液为出峰时间20~30min的洗脱段。
进一步地,将槐米水提液在25℃下静置24h,得到芦丁粗品析出物。
本发明有益效果为:以槐米为原料建立了芦丁快速、环保、有效降低成本的制备方法,为其提供了有效的资源可持续保障。
附图说明
图1为25℃槐米水提液析出物高效液相色谱;
图2为芦丁对照品高效液相色谱图;
图3为槐米水提液析出物制备液相谱图;
图4为槐米水提液析出物制备成分和芦丁对照薄层色谱图,1-槐米水提液析出物制备成分;2-芦丁对照品;
图5为槐米水提液析出物制备成分和芦丁对照高效液相色谱图。
具体实施方式
为了使本领域的人员更好地理解本发明的技术方案,下面对本发明的技术方案进行清楚、完整的描述,基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的其他类同实施例,都应当属于本申请保护的范围。
本发明实施例中槐米购于浙江中医药大学中药饮片有限公司,批号为220301;芦丁对照品(100080-202012中国食品药品检定研究院)、槲皮素对照品(100081-201610中国食品药品检定研究院)。
实施例1
(1)精密称定2g槐米粗粉,分别加入15倍量水加热回流1h,过滤,将滤液置于不同温度条件下(20℃、25℃、30℃、4℃、0℃、-18℃)放置24h,得到不同温度下槐米水提液芦丁粗品析出物,将析出物过滤、干燥、称重,计算不同放置温度下芦丁粗品析出物的得率:得率(%)=析出物重量/槐米粉末重量*100,30℃、25℃、20℃、4℃、0℃、-18℃的得率分别为12.40%、13.22%、9.96%、11.20%、10.56%、6.95%。
(2)槐米水提液芦丁析出物芦丁含量测定:精密称定10mg置于不同温度条件下(30℃,25℃,20℃,4℃,0℃、-18℃)槐米水提液芦丁粗品析出物,加适量甲醇溶解,配成浓度为0.1mg/ml的供试品溶液,将该供试品溶液进行HPLC测定分析并计算其芦丁含量,色谱条件:色谱柱为Zafex JX-C18(250 ⅹ4.6mm,5µm);流动相为甲醇-0.4%磷酸水,梯度洗脱,见表1,进样量5µL,流速1ml/min,柱温30℃,检测波长360nm。25℃下芦丁粗品槐米析出物HPLC图谱见图1,图中标号1为芦丁。芦丁对照品HPLC图谱见图2。30℃、25℃、20℃、4℃、0℃、-18℃条件下槐米水提液析出物中芦丁的含量分别是88.78%、84.65%、82.54%、85.69%、89.05%、89.23%。
表1槐米梯度洗脱程序
因此,槐米水提液芦丁粗品析出物为25℃下的槐米水提液析出物芦丁得率和纯度较高。
实施例2
(1)芦丁的制备:将实施例1中的槐米水提液芦丁粗品析出物的制备溶液注入制备型高效液相仪,制备溶液的制备方法为:精密称定槐米水提液芦丁粗品析出物10mg,加适量甲醇溶解,配成浓度为0.5mg/ml的供试品溶液,色谱柱为CTS C18 Media:12nm 10μm,进样量为0.3mL,检测波长为360nm,洗脱梯度为甲醇:水(40:60),流速为6mL·min-1,芦丁出峰时间为20~30min。在进样20min时,样品中芦丁出峰,此时将洗脱液留存,出峰结束后停止接洗脱液。将洗脱液进行浓缩,得制备芦丁样品,槐米水提液芦丁粗品析出物制备型高效液相图见图3。
(2)芦丁的确认:
①取适量芦丁对照品加甲醇制成1ml含1mg的对照品,将收集并浓缩的芦丁制备液与芦丁对照品点于同一硅胶G薄层板,按照2020年版《中国药典》一部槐花项下薄层展开条件展开,显色,结果制备的芦丁与芦丁对照品在相同位置显相同颜色的荧光斑点,确定分离得到的成分为芦丁,两者薄层色谱图见图4;
②取适量芦丁对照品,加甲醇配成浓度为0.1mg/mL的对照品溶液,将制备的芦丁与对照品溶液均按表1HPLC色谱条件进行分析,结果发现两者的保留时间一致,因此确定分离的成分为芦丁,通过计算,所得芦丁的纯度为98.62%,两者的高效液相色谱图见图5,其中S1为芦丁对照,S2为制备芦丁。根据制备芦丁的HPLC谱图发现,制得的芦丁较纯净,因此利用该方法制备分离的芦丁有较大推广价值。
Claims (5)
1.一种基于槐米水提液快速制备高纯度芦丁的方法,其特征在于,将槐米水提液在4~30℃下静置12~36h,过滤、干燥获得芦丁粗品析出物,利用制备型高效液相技术分离得到芦丁;
制备型高效液相技术具体为:将芦丁粗品析出物用甲醇溶解,注入制备型高效液相色谱仪,选取芦丁段洗脱液,得到芦丁;所述的高效液相色谱条件为色谱柱:Zafex JX-C18,250 ×4.6mm,5µm;流动相:甲醇-0.4%磷酸水梯度洗脱,进样量5µL,流速1ml/min,柱温30℃,检测波长360nm。
2.根据权利要求1所述的基于槐米水提液快速制备高纯度芦丁的方法,其特征在于,所述的槐米水提液的制备方法为:取适量槐米粗粉,加入一定10~20倍质量的水加热回流0.5~1.5h,过滤,获得槐米水提液。
3.根据权利要求1所述的基于槐米水提液快速制备高纯度芦丁的方法,其特征在于,所述的甲醇-0.4%磷酸水梯度洗脱程序为:
。
4.根据权利要求1所述的基于槐米水提液快速制备高纯度芦丁的方法,其特征在于,所述的芦丁段洗脱液为出峰时间20~30min的洗脱段。
5.根据权利要求1所述的基于槐米水提液快速制备高纯度芦丁的方法,其特征在于,将槐米水提液在25℃下静置24h,得到芦丁粗品析出物。
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