CN109470810A - 一种马缨丹药材的检测方法 - Google Patents
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Abstract
本发明提供了一种马缨丹药材的检测方法,其方法为:吸取供试品溶液、对照药材溶液2~5μl,分别点于薄层板上,以甲苯‑乙酸乙酯‑甲酸混合溶液为展开剂展开,取出,晾干,喷以显色剂,置105℃烘烤至斑点显色清晰,供试品色谱中,在与对照药材色谱相应位置上,检测对比是否显相同颜色的斑点。本方法操作简便,分离效果快速、准确,重现性良好,专属性强。
Description
技术领域
本发明属于属于中药技术领域,具体涉及一种马缨丹药材的检测方法。
背景技术
马缨丹(Lantana camara Linn.)又名五色梅、臭草、杀虫花、五彩花、如意草、山大丹等,属马鞭草科马缨丹属植物,原产巴西等地,现广泛分布于热带和亚热带各地。民间有用马缨丹治疗感冒高热、筋伤、皮炎、湿疹痉痒、腹痛吐泻、肺结核咳血等。其化学成分主要由三萜类、环烯醚萜类、黄酮类和苯丙素类等。现代药理活性表明其具有抗炎、抗菌抗病毒、抗肿瘤、降血糖和驱虫等作用。目前,对马缨丹的质量控制采用的色谱手段主要有TLC法(海南省食品药品监督管理局关于颁布我省地产马缨丹和蜂窝草中药材质量标准的通知)、GC-MS法(周晔.马缨丹挥发油的化学成分分析[J].亚太传统医药,2009,5(7):25-28.)、UV法(朱峰.紫外分光光度法测定五色梅马缨丹烯A含量研究[A].中国化学会、国家自然科学基金委员会.中国化学会第9届天然有机化学学术会议论文集[C].中国化学会、国家自然科学基金委员会:2012:1.)、HPLC法(韦会平,赵牧,阎妍,等.HPLC法测定紫茎泽兰和五色梅中β-榄香烯的含量[J].中国药房,2012,23(39):3709-3711.)。
现行标准中(海南省食品药品监督管理局关于颁布我省地产马缨丹和蜂窝草中药材质量标准的通知),马缨丹药材的TLC鉴别方法拖尾严重,斑点不清晰,不能很好的控制马缨丹药材的质量。因此急需一种更有效的马缨丹药材的TLC鉴别方法。
发明内容
本发明提供了一种马缨丹药材的检测方法。该方法操作简便,分离效果快速、准确,重现性良好,专属性强,本发明技术方案如下:
马缨丹药材的检测方法,包括以下步骤:
(1)供试品溶液的制备:
取本品粉末2~5g,加乙醇10~25ml,超声处理25~45分钟,滤过,滤液蒸干,残渣加2~4ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2~5g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2~5μl,分别点于薄层板上,以体积比为6~8.5:2.5~3.5:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
本发明所述的马缨丹药材检测方法优选为:
(1)供试品溶液的制备:
取本品粉末2g,加乙醇10ml,超声处理30分钟,滤过,滤液蒸干,残渣加2ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2μl,分别点于薄层板上,以体积比为6~8.5:2.5~3.5:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
进一步的,所述薄层板为硅胶G薄层板。
进一步的,所述展开剂甲苯-乙酸乙酯-甲酸混合溶液的体积比为7:3:0.1。
本发明的有益效果:
(1)改善了马缨丹药材的现行标准中TLC鉴别方法拖尾严重,斑点不清晰,不能很好的控制马缨丹药材的质量的技术问题;
(2)本方法操作简便,分离效果快速、准确,重现性良好,专属性强,能够作为马缨丹药材的质量控制方法。
附图说明
图1是实施例1-2的马缨丹薄层鉴别图,其中1-实施例1对照药材样品;2-实施例1供试品溶液样品;3-实施例2对照药材样品;4-实施例2供试品溶液样品。
图2是实施例3-4的马缨丹薄层鉴别图,其中1-实施例3对照药材样品;2-实施例3供试品溶液样品;3-实施例4对照药材样品;4-实施例4供试品溶液样品。
图3是对比例1的马缨丹药材薄层鉴别图,其中1-对比例1对照药材样品;2-对比例1供试品溶液样品;3-对比例1供试品溶液样品;4-对比例1供试品溶液样品。
图4是对比例1的马缨丹药材薄层鉴别图,为置于紫外灯(365nm)下检视的薄层鉴别图,其中1-对比例1对照药材样品;2-对比例1供试品溶液样品;3-对比例1供试品溶液样品;4-对比例1供试品溶液样品。
具体实施方式
实施例1
一种马缨丹药材的检测方法,包括以下步骤:
(1)供试品溶液的制备:
取本品粉末2g,加乙醇10ml,超声处理30分钟,滤过,滤液蒸干,残渣加2ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2μl,分别点于薄层板上,以体积比为7:3:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
检测结果:供试品色谱中,在与对照药材色谱相应位置上,显相同颜色的斑点;斑点清晰,无拖尾。见附图1。
实施例2
一种马缨丹药材的检测方法,包括以下步骤:
(1)供试品溶液的制备:
取本品粉末2g,加乙醇15ml,超声处理45分钟,滤过,滤液蒸干,残渣加3ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2μl,分别点于薄层板上,以体积比为7:3:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
检测结果:供试品色谱中,在与对照药材色谱相应位置上,显相同颜色的斑点;斑点清晰,无拖尾。见附图1。
实施例3
一种马缨丹药材的检测方法,包括以下步骤:
(1)供试品溶液的制备:
取本品粉末3g,加乙醇15ml,超声处理25分钟,滤过,滤液蒸干,残渣加4ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材3g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取5μl,分别点于薄层板上,以体积比为8:3:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
检测结果:供试品色谱中,在与对照药材色谱相应位置上,显相同颜色的斑点;斑点清晰,无拖尾。见附图2。
实施例4
一种马缨丹药材的检测方法,包括以下步骤:
(1)供试品溶液的制备:
取本品粉末3g,加乙醇20ml,超声处理40分钟,滤过,滤液蒸干,残渣加4ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材3g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取5μl,分别点于薄层板上,以体积比为8:3:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
检测结果:供试品色谱中,在与对照药材色谱相应位置上,显相同颜色的斑点;斑点清晰,无拖尾。见附图2。
对比例1
一种马缨丹药材的检测方法,包括以下步骤:
取本品粉末2g,加乙醇10ml,超声处理30分钟,滤过,滤液蒸干,残渣加2ml乙醇使溶解。另取马缨丹对照药材2g,同法制成对照药材溶液。照薄层色谱法(中国药典2015年版四部通则0502)试验,吸取上述两种溶液各10μl,分别点于同一硅胶G薄层板上,以乙酸乙酯-丙酮-甲酸-水(5:5:1:1)为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,在105℃加热至斑点显色清晰,供试品色谱中,对比检测在与对照药材色谱相应位置上,是否显相同颜色的斑点;置紫外灯(365nm)下检视,供试品色谱中,对比检测在与对照药材色谱相应位置上是否显相同颜色的荧光斑点。
检测结果:拖尾严重,斑点不清晰,见附图3、4。
Claims (4)
1.一种马缨丹药材的检测方法,其特征在于包括以下步骤:
(1)供试品溶液的制备:
取本品粉末2~5g,加乙醇10~25ml,超声处理25~45分钟,滤过,滤液蒸干,残渣加2~4ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2~5g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2~5μl,分别点于薄层板上,以体积比为6~8.5:2.5~3.5:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
2.根据权利要求1所述的方法,其特征在于包括以下步骤:
(1)供试品溶液的制备:
取本品粉末2g,加乙醇10ml,超声处理30分钟,滤过,滤液蒸干,残渣加2ml乙醇使溶解,作为供试品溶液;
(2)对照药材溶液的制备:
取马缨丹对照药材2g,同步骤(1)方法制成对照药材溶液;
(3)薄层色谱法鉴别:
吸取步骤(1)-(2)中供试品溶液、对照药材溶液等体积量,各吸取2μl,分别点于薄层板上,以体积比为6~8.5:2.5~3.5:0.1的甲苯-乙酸乙酯-甲酸混合溶液为展开剂,展开,取出,晾干,喷以10%硫酸乙醇溶液,置105℃烘烤至斑点显色清晰;供试品色谱中,在与对照药材色谱相应位置上,对比是否显相同颜色的斑点。
3.根据权利要求1或2所述的方法,其特征在于,所述薄层板为硅胶G薄层板。
4.根据权利要求1或2所述的方法,其特征在于,所述展开剂甲苯-乙酸乙酯-甲酸混合溶液的体积比为7:3:0.1。
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