張盈嬌++夏陳++陳建
摘要 [目的]建立獸藥三黃散超微粉中黃芩苷和鹽酸小檗堿含量的高效液相色譜法測定方法。[方法]采用十八烷基硅烷鍵合硅膠柱ZORBAX Eclipse XB-C18(4.6 mm×250 mm,5 μm)為色譜柱,黃芩苷和鹽酸小檗堿的檢測波長分別為278 nm和347 nm,流動相:乙腈-2 mL/L磷酸水溶液(體積比25∶75),柱溫30 ℃;流速1.0mL/min,進樣量10 μL。[結果]黃芩苷、鹽酸小檗堿進樣量分別在0.1180~1.1800、0.051 6~0.516 0 μg(R2=0.999,n=6)范圍內與其各自峰面積積分值呈良好的線性關系,平均加樣回收率分別為101.696%、100.604%(n=6)。[結論]此方法精確、快速,重現性和精密度良好,可為獸藥三黃散超微粉的質量控制及質量標準的建立提供技術支撐。
關鍵詞 三黃散超微粉;黃芩苷;鹽酸小檗堿;高效液相色譜法
中圖分類號 S853.74 文獻標識碼 A 文章編號 1007-5739(2015)18-0266-02
Simultaneous Determination of Baicalin and Berberine Hydrochloride in Sanhuang San for Animals by HPLC
ZHANG Ying-jiao XIA Chen CHEN Jian *
(Institute of Agro-food Science and Technology,Sichuan Academy of Agricultural Sciences,Chengdu Sichuan 610066)
Abstract [Objective] To establish a HPLC method for simultaneous determination of baicalin and berberine hydrochloride in Sanhuang San of veterinary drugs.[Method] The content determination was performed on ZORBAX Eclipse XB-C18(4.6 mm×250 mm,5 μm),with the mobile phase consisted of acetonitrile-2 mL/L phosphoric acid(25∶75).The flow rate was 1.0 mL/min,and the detection wavelength of baicalin and berberine hydrochloride was set at 278 nm and 347 nm.The column temperature was maintained at 30 ℃ and injection volume was 10 μL.[Results] The linear range of baicalin and berberine hydrochloride were from 0.1180 to 1.1800 μg(R2=0.999,n=6)and from 0.051 6 to 0.516 0 μg(R2=0.999,n=6),respectively,and the average recoveries were 101.696% and 100.604%(n=6),respectively.[Conclusion] The method was simple,accurate,re-producible and precise,which would be suitable for contents determination,quality control and evaluation of baicalin and berberine hydrochloride in Sanhuang San of veterinary drugs.
Key words Sanhuang San;baicalin;berberine hydrochloride;HPLC
獸藥三黃散超微粉主要由黃柏、黃芩、大黃等組成,主治細菌性敗血癥、爛鰓、腸炎和赤皮,適用于各類水產養殖動物[1]。黃芩苷(baicalin)和鹽酸小檗堿(berberine hydrochloride)是主要有效成分,黃芩苷是一種黃酮類化合物,具有抑菌、利尿、抗炎、抗變態及解痙作用,在清除氧自由基、減輕組織的缺血、促進細胞凋亡等多方面均有作用[2-3]。鹽酸小檗堿是一種異喹啉生物堿,又稱黃連素(umbellatine),對痢疾桿菌、大腸桿菌、肺炎雙球菌等有抑制作用,主要用于胃腸道感染及菌痢等[4-5]。顯然,黃芩苷、鹽酸小檗堿含量高低直接影響三黃散超微粉的藥效。
超微粉碎技術可將中藥材粉碎到粒徑1~75 μm,是近年來中藥加工的一項新技術,該技術改善了中藥的品質,提高了中藥的生物利用度,推動了中藥的標準化,是中藥現代化的重要途徑之一?!?br>