半夏泻心汤胃内滞留片质量标准的研究  

Study on quality control of Banxia Xiexin Decoction gastric floating sustained-release tablets

作　　者：杨志欣[1] 李晓阳[1] 王祺茹 李霞[1] 单柏松 刘佳佳[1] 邓伟哲[2] 

机构地区：[1]黑龙江中医药大学药学院,黑龙江哈尔滨150040 [2]中国人民解放军第211医院中医科,黑龙江哈尔滨150080

出　　处：《上海中医药杂志》2016年第5期93-96,共4页Shanghai Journal of Traditional Chinese Medicine

基　　金：国家教育部春晖计划资助项目(Z2008-1-15016);黑龙江中医药大学"优秀创新人才支持计划"项目(2012)

摘　　要：目的建立半夏泻心汤胃内滞留片质量控制方法。方法采用薄层色谱法对方中黄芩、黄连定性鉴别,高效液相色谱法定量分析黄芩苷、盐酸小檗碱的含量及体外药物释放。Diamonsil C_(18)色谱柱,黄芩苷以甲醇-水-磷酸(47∶53∶0.2)等度洗脱,280 nm波长处检测;盐酸小檗碱以乙腈-0.05 mol/L磷酸二氢钾(50∶50)等度洗脱,345 nm波长处检测。结果半夏泻心汤胃内滞留片中黄芩、黄连中的黄芩苷、盐酸小檗碱在薄层色谱中有良好的分离度。黄芩苷和盐酸小檗碱的线性回归方程分别为Y=40 763X-54 322(R^2=0.999 1)和Y=624 71X-163 59(R^2=0.999 7),分别在4~20 mg/L和5~25 mg/L范围内线性关系良好,方法学考察均符合要求。测定6批半夏泻心汤胃内滞留片中黄芩苷和盐酸小檗碱的含量分别为(19.95±0.72)mg/片和(13.02±1.05)mg/片。体外10 h释药达90%以上,确定体外释药时间点为2、6、10 h。结论本研究所建立的定性、定量分析方法灵敏可靠、简便、精密度高、重现性好,体外释放取样点的确定符合《药典》要求,可用于半夏泻心汤胃内滞留片的质量控制。Objective To develop a new, simple and reproducible method for the quality control of Banxia Xiexin Decoction gastric retention tablets. Methods TLC was performed for qualitative identification of Scutellaria baicalensisand and Rhizoma Coptidis. HPLC was used for the quantitative analysis of drug release in vitro and determination of baicalin and berberine hydrochloride. Baicalin was quantified on a Diamonsil Cls column using a mixture of methanol-water-phosphoric （47：53：0.2, v/v/v） as the mobile phase with UV detection at 280 nm, and berberine hydrochloride was quantified,＇ using acetonitrile- 0. 05 mol/L potassium dihydrogen phosphate （50：50, v/v） as the mobile phase with UV detection at 345 nm. Results Calibration curves were linear in the concentration range of 4 ~ 20 i^g/mL of baicalin （ Y = 40763X - 54322, R2 = 0. 9991 ） and of 5 ~ 25 txg/mL of berberine hydrochloride （ Y = 62471X - 16359, R2 = 0. 9997 ）, respectively. The results of methodology study were in line with the requirements. The content of baicalin and berberine hydrochloride was validated to be 19.95 ＋ 0.72mg / tablet and 13.02 ＋ 1.05 mg / tablet by determining six batches of Banxia Xiexin Dectotion gastric retention tablets. The release time was confirmed to be 2h, 6h and 10h. After 10h, the release rate was greater than 90%. Conclusion A sensitive, reliable, easy and reproducible method was established for qualitative and quantitative analysis of Banxia Xiexin Decoction gastric retention tablets, with the sampling point in accordance with Pharmacopoeia. The method is suitable for the quality control of Banxia Xiexin Decoction gastric retention tablets.

关 键 词：半夏泻心汤 胃内滞留片 盐酸小檗碱 黄芩苷 薄层色谱 高效液相色谱法 质量控制 

分 类 号：R286.0[医药卫生—中药学]