杜仲降压片质量控制方法研究

发布时间：2018-11-17 09:33

【摘要】：杜仲降压片由杜仲、益母草、夏枯草、黄芩、钩藤5味中药组成,最早收载于《中国药典》1977年版一部,为糖衣片,检测项目只有钩藤的显微鉴别和理化鉴别,无含量测定项。1992年收载于《卫生部药品标准》中药成方制剂第6册,标准编号为WS3-B-1185-92,名称改为复方杜仲片(杜仲降压片),为糖衣片,处方与《中国药典》1977年版相同,但对制法做了修改,检测项目只有钩藤的显微鉴别和理化鉴别,无含量测定项。2014年广州市香雪制药股份有限公司对复方杜仲片(杜仲降压片)修改了规格,标准为国家药品标准YBZ28882005(WS3-B-1185-92-1),为薄膜衣片,检测项目只有钩藤的显微鉴别和理化鉴别,无含量测定项。2015年康普药业股份有限公司对复方杜仲片的标准进行了提高,质量标准为国家食品药品监督管理局国家药品标准YBZ07792004(WS3-B-1185-92-2),检验项目新增了盐酸水苏碱、熊果酸的薄层色谱鉴别和用高效液相色谱法测定黄芩苷含量。杜仲降压片具有补肾、平肝、清热之功效,用于肾虚肝旺之高血压症。目前关于杜仲降压片质量控制方法的研究较少,因此建立对其的质量控制方法至关重要。杜仲补肝肾、强筋骨、安胎等功效。益母草活血调经,利尿消肿清热解毒。夏枯草清肝泻火,明目,散结消肿。黄芩清热燥湿,泻火解毒,止血,安胎。钩藤息风定惊,清热平肝。本研究建立了杜仲降压片中杜仲、益母草、钩藤的薄层色谱鉴别方法,夏枯草中迷迭香酸、黄芩中黄芩苷及黄芩素的高效液相色谱含量测定方法及杜仲降压片中杜仲、益母草、夏枯草、黄芩、钩藤5味中药材的特征图谱研究方法。目的:建立杜仲降压片的质量控制方法。方法:薄层色谱法鉴别杜仲降压片中的杜仲、益母草、钩藤;高效液相色谱法测定夏枯草中迷迭香酸及黄芩中黄芩苷和黄芩素的含量,并对杜仲降压片特征图谱进行了研究,色谱柱为Thermo(赛默飞)(4.6×250mm;5μm),乙腈-0.1%磷酸溶液梯度洗脱,流速为1.0 mL·min-1,检测波长为330 nm,柱长250mm,柱温为30℃。结果:薄层色谱中,在与杜仲对照药材、盐酸水苏碱对照品、钩藤对照药材相应的位置上,显相同颜色的斑点。建立了杜仲降压片中杜仲、益母草、夏枯草、黄芩、钩藤5味中药材的特征图谱,共有8个特征峰,以峰6为S峰,各特征峰的相对保留时间分别为0.37、0.48、0.51、0.59、0.95、1.00、1.40、1.46。迷迭香酸在49.9~898.6μg范围内,线性关系良好,回归方程为Y=3086.1x+2607.1,R2=1,黄芩苷在355.2~6776.0μg范围内,线性关系良好,回归方程为Y=1656.8 x-145198,R2=0.9996,黄芩素在83.5~453.6μg范围内,线性关系良好,回归方程为Y=2827.8x-24929,R2=0.9998。方法重复性、精密度、稳定性、耐用性良好,回收率分别为101.7%、98.1%、97.6%,RSD2%。结论:本研究中建立的方法快捷高效,专属性良好,能较好地控制杜仲降压片的质量。
[Abstract]:Kuzhong Jiangya tablet is composed of five kinds of Chinese medicine, Eucommia ulmoides, Leonurus, Prunella subtilis, Scutellaria baicalensis, Uncaria, which was first collected in 1977 edition of the Chinese Pharmacopoeia. It is a sugar-coated tablet. No content determination item. 1992 in the "Ministry of Health Drug Standards" Chinese medicine prescription, Volume 6, the standard number for WS3-B-1185-92, changed to compound Eucommia tablets (Duzhong Jiangya tablets), as a sugar coating tablets, The prescription was the same as the 1977 edition of Chinese Pharmacopoeia, but the preparation method was modified. In 2014, Guangzhou Xiangxue Pharmaceutical Co., Ltd. revised the specification of compound Eucommia ulmoides tablets (Duzhong Jiangya tablets), the national drug standard YBZ28882005 (WS3-B-1185-92-1), the film clothing tablets, In 2015, Kangpu Pharmaceutical Co., Ltd. improved the standard of compound Eucommia tablets. The quality standard is YBZ07792004 (WS3-B-1185-92-2), the national drug standard of the State Food and Drug Administration. The TLC identification of stachydrine hydrochloride and ursolic acid and the determination of baicalin by high performance liquid chromatography (HPLC) have been added to the test item. Duzhong Jiangya tablet has the effect of tonifying kidney, calming the liver and clearing heat. There are few researches on the quality control methods of Eucommia ulmoides hypotensive tablets at present, so it is very important to establish the quality control methods for Eucommia ulmoides. Eucommia tonify liver and kidney, strengthen muscles and bones, and so on. Motherwort grass blood-activating regulation, diuretic swelling-clearing-heat detoxification. Prunus vulgaris clear the liver, clear the fire, eyes, scattered knot detumescence. Scutellaria clear heat and dampness, diarrhea fire detoxification, hemostasis, Anti-fetus. Hookwood wind calm alarm, clearing heat and calming the liver. In this study, a TLC method for identification of Eucommia ulmoides, Leonurus and Uncaria in Kuzhong Jiangya tablets, determination of rosemary acid in Prunella vulgaris, baicalin and baicalin in Scutellaria baicalensis, and Eucommia ulmoides and Leonurus in Jiangya tablets of Eucommia ulmoides were established. Study on characteristic Atlas of five Chinese Medicinal herbs, Prunella subtilis L., Scutellaria baicalensis and Rhizoma Uncaria. Objective: to establish a quality control method for Eucommia uzhong Jiangya tablets. Methods: TLC was used to identify Eucommia ulmoides, Leonurus and Uncaria in Jiangya tablets of Eucommia ulmoides. The content of rosemary acid, baicalin and baicalin in Scutellaria baicalensis was determined by HPLC. The characteristic chromatogram of Eucommia ulmoides Jiangya tablets was studied. The chromatographic column was Thermo (4.6 脳 250mm). The gradient elution of 5 渭 m), acetonitrile-0.1% phosphoric acid solution was carried out at a flow rate of 1.0 mL min-1,. The detection wavelength was 250 mm at 330 nm, and the column temperature was 30 鈩，

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