目的确定肠激安制剂(白芍、黄连、白术、防风等)中芍药苷、盐酸巴马汀及盐酸小檗碱测定方法。方法采用高效液相色谱法,以Kromat universal C18(4.6 mm×250 mm,5μm)色谱柱用于芍药苷测定、Eclipse XDB-C18(4.6 mm×250mm,5μm)色谱柱用于盐酸巴马汀和盐酸小檗碱测定,分别用乙腈-0.1%磷酸溶液(15∶85)、乙腈-0.05 mol/L磷酸二氢钾溶液(50∶50)为流动相。体积流量均为1.0 mL/min;检测波长分别为230 nm、345 nm;柱温分别为25℃、20℃。结果芍药苷、盐酸巴马汀和盐酸小檗碱峰分离度好,且在0.102 02~0.816 16μg、0.027 9~0.139 4μg和0.111 5~0.557 5μg范围内线性关系良好,平均回收率分别为为99.82%、101.06%和100.23%,RSD值分别为1.71%、1.97%和1.92%(n=9),其精密度、稳定性以及重复性良好。结论高效液相色谱法是该提取物中这3种成分定量测定的简单有效的方法,为今后的研究奠定了基础。
AIM To establish an HPLC method for determining the contents of paeoniflorin,palmatine hydrochloride and berberine hydrochloride in Changji'an Preparation(Paeoniae Radix alba,Coptidis Rhizoma,Atractylodis macrocephalae Rhizoma,Saposhnikoviae Radix,etc.).METHODS HPLC was used.The Kromat universal C18 column was adopted with acetonitrile-0.1% phosphoric acid solution(15∶ 85) for the determination of paeoniflorin and the clipse XDB-C18 column was adopted with acetonitrile-0.05 mol/L potassium dihydrogen phosphate(50∶ 50)for the determination of palmatine hydrochloride and berberine hydrochloride.The flow rate was 1.0 mL/min and the detection wavelengths were set at 230 nm and 345 nm,respectively.The column temperatures were maintained at 25 ℃,20 ℃,respectively.RESULTS The separations of paeoniflorin,palmatine hydrochloride and berberine hydrochloride peaks were good.The calibration curves were linear in the ranges of 0.102 02-0.816 16 μg for paeoniflorin,0.027 9-0.139 4 μg for palmatine hydrochloride and 0.111 5-0.557 5 μg for berberine hydrochloride.The average recoveries were 99.82%,101.06% and 100.23%,respectively.The RSDs were 1.71%,1.97% and 1.92%(n=9),respectively.The precision,stability and reproducibility were good.CONCLUSION This method is simple,efficient,and can guide the research in future.