目的 建立追风透骨丸中α-香附酮和香附烯酮含量测定的高效液相色谱法(HPLC).方法 色谱条件采用色谱柱ZORBAX SB-C18(4.6×250 mm,5 μm),以甲醇(A)-水(B)(65∶35)为流动相,流速为1.0 ml/min,柱温为30℃,检测波长为254 mn,进样量为5 μl.结果 α-香附酮、香附烯酮检测质量线性范围分别为0.080 36~0.803 6 μg、0.211 2~2.112 μg,(r均为1.000);平均加样回收率分别为102.0%、101.5%,相对标准偏差(RSD)分别为1.6%、1.4%(n均等于6);精密度、稳定性、重复性的 RSD 均小于 2.0%(n=6).结论 建立的质量控制方法简便、准确、可靠、专属性好,可用于追风透骨丸中α-香附酮和香附烯酮的含量测定,为追风透骨丸中香附(制)质量控制提供依据.
Objective To establish High performance liquid chromatography(HPLC)for the determination of a-Xiangfu ketone and Xiangfu enone in Zhuifeng Tougu pills.Methods The chromatographic conditions were determined using a chromatographic column ZORBAX SB-C18(4.6 mm×250 mm,5 μm)Using methanol(A)-water(B)(65:35)as the mobile phase,the flow rate is 1.0 ml/min,the column temperature is 30℃,the detection wavelength is 254 mn,and the injection amount is 5 μl.Results α-The linear range of detection quality for Xiangfu ketone and Xiangfu enone is 0.080 36~0.803 6 μg,0.211 2 μg~2.112 μg(r=1.000);The average spiked recovery rates were 102.0% and 101.5%,respectively,with RSDs of 1.6% and 1.4%(n=6);The RSD of precision,stability,and repeatability are all less than 2.0%(n=6).Conclusion The established quality control method is simple,accurate,reliable,and has good specificity.It can be used for the determination of a-Xiangfu ketone and Xiangfu enone in Zhuifeng Tougu pills,providing a basis for the quality control of Xiangfu(preparation)in Zhuifeng Tougu pills.