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目的建立同时测定当归补血汤中三种指标性成分——阿魏酸、毛蕊异黄酮葡萄糖苷和黄芪甲苷含量的HPLCDAD/ELSD法。方法使用Agilent ZORBAX Eclipse XDB-C18色谱柱,柱温为30℃。流动相A:0.2%甲酸溶液,流动相B:0.2%甲酸乙腈溶液,梯度洗脱:0~10min,15%-20%B;10~20min,20%~40%B,20~30min,40%B,流速为1ml/min;进样量为10μl;DAD和ELSD串联测定,其中DAD检测波长分别为316nm和260nm;ELSD参数设定为蒸发温度:30℃,雾化温度:30℃,气体流速:1.6L/min。结果阴性对照无干扰,阿魏酸、毛蕊异黄酮葡萄糖苷和黄芪甲苷的线性范围分别为1.5~60μg/ml(r=1.0000),12.5~400μg/ml(r=0.9998)和0.25~2.5mg/ml(r=0.9975);其平均加样回收率分别为103.68%、102.95%和98.19%。结论所建含量测定方法简便、准确和可靠,可作为当归补血汤质量控制的标准。
OBJECTIVE To establish an HPLCDAD / ELSD method for the simultaneous determination of three major components in the Danggui Buxue Tang - ferulic acid, calycosin glucoside and astragaloside. Method The Agilent ZORBAX Eclipse XDB-C18 column was used with a column temperature of 30 ° C. Mobile phase A: 0.2% formic acid solution, mobile phase B: 0.2% formic acid in acetonitrile, gradient elution: 0-10 min, 15-20% B; 10-20 min, 20-40% B, % B, the flow rate was 1ml / min; injection volume was 10μl; DAD and ELSD were measured in series with DAD detection wavelength at 316nm and 260nm respectively; ELSD parameters were set at evaporation temperature of 30 ℃, atomization temperature of 30 ℃, gas Flow rate: 1.6 L / min. Results The negative control had no interference. The linear ranges of ferulic acid, calycosin glucoside and astragaloside were 1.5-60μg / ml (r = 1.0000), 12.5-400μg / ml (r = 0.9998) and 0.25-2.5mg / ml (r = 0.9975). The average recoveries were 103.68%, 102.95% and 98.19%, respectively. Conclusion The determination method of content is simple, accurate and reliable, which can be used as the quality control standard of Danggui Buxue Decoction.