摘要
目的建立反相高效液相色谱法定量测定8家企业生产的逍遥丸中芍药苷、游离苯甲酸和苯甲酰基总苷。方法逍遥丸甲醇提取液分析采用Agilent Eclipse XDB C18色谱柱（4.6 mm×250 mm,5μm）,测定芍药苷和苯甲酸的流动相为乙腈（A）-0.1%磷酸溶液（B）,梯度洗脱;苯甲酰基总苷以总苷碱水解为苯甲酸计算,色谱条件同上。结果芍药苷和游离苯甲酸进样量分别在0.060 8-0.760μg（r=0.999 8）、0.009 6-0.120 0μg（r=0.999 7）范围内与峰面积线性关系良好,平均回收率（n=6）为97.3%（RSD=2.2%）和97.2%（RSD=2.2%）;苯甲酰基总苷在0.020 32-0.304 8μg范围内线性关系良好（r=0.999 6）,平均回收率（n=6）为96.6%（RSD=2.8%）。结论建议增加苯甲酰基总苷的定量测定可有助于更好地控制逍遥丸的内在质量。
AIM To establish an HPLC method for determining the contents of paeoniflorin,free benzoic acid,and total benzoyl glucosides（ with benzoic acid as control） in Xiaoyao（ water） Pills produced by eight manufactories. METHODS The analysis of Xiaoyao Pills methanolic extract was performed on Agilent Eclipse XDB C18column（ 4. 6 mm × 250 mm,5 μm）. The mobile phase for simultaneous determining paeoniflorin and benzoic consisted of acetonitrile（ A）-0. 4% phosphoric acid（ B） in gradient elution mode at the flow rate of 1. 0m L / min. The detection wavelength was set at 230 nm. Using the method of alkaline hydrolysis,the total benzoyl glucosides in Xiaoyao Pills were hydrolyzed into benzoic acid,determined by HPLC,and calculated as benzoic acid content. The chromatographic conditions were the same as the above. RESULTS The linear ranges of paeoniflorin and free benzoic acid were in the ranges of 0. 060 8- 0. 760 μg（ r = 0. 999 8） and 0. 009 6- 0. 120 0 μg（ r =0. 999 7）,respectively. The average recovery rates（ n = 6） were 97. 3%（ RSD = 2. 2%） and 97. 2%（ RSD =2. 2%）,respectively. The linear range of benzoyl glucosides was in the ranges of 0. 020 32- 0. 304 8 μg（ r =0. 999 6）,and the average recovery rate（ n = 6） was 96. 6%（ RSD = 2. 8%）. CONCLUSION The method is simple,accurate and sensitive,and can be used for the quality control of Xiaoyao Pills.
出处
《中成药》
CAS
CSCD
北大核心
2015年第8期1722-1727,共6页
Chinese Traditional Patent Medicine
