作 者: (曾桢); (艾光丽); (李婷婷); (文永盛); (周世玉);
机构地区: 成都市食品药品检验研究院,成都610045
出 处: 《中国药房》 2017年第24期3405-3408,共4页
摘 要: 目的:建立同时测定小儿化毒散中芍药苷、盐酸小檗碱、甘草酸铵含量的方法。方法:采用高效液相色谱法。色谱柱为Waters SunFire^(TM)-C_(18),流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为238 nm,柱温为25℃,进样量为10μL。结果:芍药苷、盐酸小檗碱、甘草酸铵检测质量浓度线性范围分别为8.808~88.08μg/mL(r=0.999 8)、1.778~17.78μg/mL(r=0.999 6)、2.533~25.33μg/mL(r=0.999 9);定量限分别为4.404、0.889、2.533μg/mL,检测限分别为1.101、0.445、1.267μg/mL;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为95.08%~99.61%(RSD=1.77%,n=9)、96.93%~99.94%(RSD=0.92%,n=9)、98.33%~102.05%(RSD=1.27%,n=9)。结论:该方法简单、准确、重复性好,可用于小儿化毒散中芍药苷、盐酸小檗碱、甘草酸铵含量的同时测定。 OBJECTIVE: To establish a method for simultaneous determination of paeoniflorin, berberine hydrochloride and ammonium glycyrrhizinate in Xiaoer huadu powder. METHODS: HPLC method was adopted. The separation was performed on Wa- ters SunFirerU-C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 238 nm, and column temperature was 25℃. The sample size was 10 μL. RE- SULTS: The linear ranges of paeoniflorin, berberine hydrochloride and ammonium glycyrrhizinate were 8.808-88.08μg/mL (r= 0.999 8), 1.778-17.78 μg/mL(r=0.999 6), 2.533-25.33 μg/mL(r=0.999 9), respectively. LOQ were 4.404, 0.889, 2.533 μg/mL; LOD were 1.101, 0.445, 1.267 μg/mL. RSDs of precision, stability and reproducibility tests were all lower than 2%. The recover- ies were 95.08%-99.61% (RSD= 1.77%, n=9), 96.93%-99.94% (RSD=0.92%, n=9), 98.33%-102.05% (RSD= 1.27%, n=9). CONCLUSIONS: The method is simple, accurate and reproducible, and can be used for simultaneous determination of paeoniflo- fin, berberine hydrochloride and ammonium glycyrrhizinate in Xiaoer huadu powder.