李筱婧 韋英杰 汪晶 許歡 黃一平 江阿古麗·艾山 陳斌



[摘要] 目的 建立瑪瑙膏的質量標準。 方法 采用薄層色譜法對制劑中五靈脂、延胡索、大黃、補骨脂、三七進行定性鑒別;采用高效液相色譜法對制劑中延胡索乙素進行含量測定,以乙腈-0.1%磷酸三乙胺體系為流動相,梯度洗脫,柱溫30℃,檢測波長280 nm。 結果 薄層色譜法斑點清晰,分離度好,陰性無干擾;延胡索乙素在2.022~20.22 μg/mL(r = 0.9999)范圍內呈良好的線性關系,平均加樣回收率為100.27%(RSD = 2.39%)。 結論 本研究建立的方法穩定性、重復性好,可用于瑪瑙膏的質量控制。
[關鍵詞] 瑪瑙膏;質量標準;薄層色譜法;高效液相色譜法;延胡索乙素
[中圖分類號] R927.1? ? ? ? ? [文獻標識碼] A? ? ? ? ? [文章編號] 1673-7210(2020)07(c)-0133-04
Quality standard for Ma′nao Gao
LI Xiaojing1? ?WEI Yingjie1,2? ?WANG Jing1,2? ?XU Huan1? ?HUANG Yiping1,2? ?Janagul·As3? ?CHEN Bin1,2
1.The Third Clinical Medical College, Nanjing University of Chinese Medicine, Jiangsu Province, Nanjing? ?210028, China; 2.Key Laboratory for Traditional Chinese Medicine Drug Release System Under State Administration of Traditional Chinese Medicine, Jiangsu Province Academy of Traditional Chinese Medicine, Jiangsu Province, Nanjing? ?210028, China; 3.Xinjiang Yili Kazak Autonomous Prefecture Hospital of Traditional Chinese Medicine, Xinjiang Uygur Autonomous Region, Yining? ?835000, China
[Abstract] Objective To establish a quality control method for Ma′nao Gao. Methods Thin layer chromatography was applied to the qualitative identification of Faeces Togopteri, Corydalis Rhizoma, Rhei Radix et Rhizoma, Psoraleae Fructus, Notoginseng Radix et Rhizoma. High performance liquid chromatography was used for the content determination of tetrahydropalmatine, acetonitrile-0.1% triethylamine phosphate system was used as the mobile phase of gradient elute. The column temperature was 30°C and the detection wavelength was set at 280 nm. Results Thin layer chromatography spots was clear, which had good resolution without interference. Tetrahydropalmatine had good linear relationship with the range of 2.022-20.22 μg/mL (r = 0.9999) respectively, the average recovery was 100.27% (RSD = 2.39%). Conclusion The method is reliable with good stability and good repeatability, and can be used for quality control of Ma′nao Gao.
[Key words] Ma′nao Gao; Quality standardization; Thin layer chromatography; High performance liquid chromatography; Tetrahydropalmatine
哈薩克民族醫藥是中國民族醫藥體系中重要的組成部分,哈薩克醫藥秘方瑪瑙膏是外敷治療外傷性腫痛的“明珠”,由五靈脂、延胡索、大黃等11味藥材組成,主要用于治療跌打損傷、四肢疼痛等血瘀癥和痹證,具有消腫止痛、活血化瘀、行氣消腫、促進骨愈合的作用,效果明確。江阿古麗等[1]通過抗炎鎮痛動物實驗研究,發現瑪瑙膏對實驗性腫痛有明顯的治療作用,表現出顯著的抗炎效果。此外,還進行了瑪瑙膏外敷治療骨與軟組織損傷的臨床研究[2],對外傷致骨及軟組織損傷患者于治療前后進行病情評分分析,結果顯示,瑪瑙膏對外傷性腫痛的消腫止痛作用明顯優于對照組(P < 0.001)。哈藥瑪瑙膏目前暫無質量標準,為適應民族藥醫院制劑制造規范化、標準化,以確保臨床療效及用藥安全,本試驗進行瑪瑙膏質量標準研究,建立瑪瑙膏中五靈脂、延胡索、大黃、補骨脂、三七的薄層色譜鑒別方法及延胡索乙素的高效液相色譜法(HPLC)含量測定方法。
2.2.7 精密度試驗? 精密吸取濃度為12.132 μg/mL的延胡索乙素對照品溶液,按照“2.2.1”項下色譜條件連續進樣6次,記錄峰面積,測定值的RSD為0.088%,結果提示精密度良好。……