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出 处:《中成药》2014年第6期1203-1208,共6页Chinese Traditional Patent Medicine
摘 要:目的建立同时测定荆防小儿止咳口服液(荆芥、防风、连翘和苦杏仁等)中升麻素苷和连翘苷的方法。方法以升麻素苷和连翘苷的量为评价指标,选择氧化铝柱和洗脱剂种类和用量。色谱条件采用Kromasil ODS1(250mm×4.6mm,5μm)色谱柱,以乙腈-水为流动相进行梯度洗脱(0~15min,16%乙腈;15~50min,22%乙腈),体积流量1.0mL/min,检测波长277nm,柱温30℃。结果氧化铝柱层析条件是用中性氧化铝干法装柱,洗脱剂为50%乙醇,洗脱体积为40mL。升麻素苷在0.0936~0.7020μg范围内线性良好(r=0.9998),平均回收率为98.88%,RSD为2.18%(n=6);连翘苷在0.1104~0.8280μg范围内线性良好(r=0.9996),平均回收率为100.55%,RSD为2.43%(n=6)。结论方法简单易行,重复性好,可用于同时测定荆防小儿止咳口服液中升麻素苷和连翘苷的含有量。AIM To establish a method for simultaneously determining the contents of prim-O-glucosylcimifu- gin and forsythin in Jingfang Children Cough Oral Liquid (Schizonepetae Herba, Saposhnikoviae Radix, Forsythiae Fructus, AmeniacaeSemen amarum, etc). METHODS The choices of Al2O3 column chromatograph and elution solvent were made among the type and use level with the content of prim-O-glucosylimfugin and forsythin as evalua- tion indexes. The HPLC analysis of samples was carried out on RP-C18 column (250 mm ×4. 6 mm, 5 μm) with acetonitrile -water (0 - 15 min, 16% aeetonitrile; 15 -50 rain, 22% acetonitrile) as moble phase in gradient e- lution manner, at a flow rate of 1.0 mL/min and detection wavelength of 277 nm, and under column temperature of 30℃. RESULTS The neutral Al2O3 column and dry column packing were chosen with 40 mL of 50% ethanol as eluting agent. The calibration curve of prim-O-glueosyleimifugin was linear in the range of 0. 093 6 ~ 0. 702 0μg (r =0. 999 8) , and the average recovery and RSD were 98.88% and 2. 18% (n =6) , respectively. The cali- bration curve of forsythin was linear in the range of 0. 110 4 ~0. 828 0 μg (r =0. 999 6) , and the average recovery and RSD were 100.55% and 2. 43% ( n = 6 ) , respectively. CONCLUSION The method is simple, feasible and reproducible, and available for simultaneous determination of above two constituents in the oral liquid.
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