HPLC波长切换技术同时测定知柏地黄丸(浓缩丸)中莫诺苷、芒果苷、马钱苷和丹皮酚的含量

目的: 建立HPLC法同时测定知柏地黄丸(浓缩丸)中莫诺苷、芒果苷、马钱苷、丹皮酚的含量. 方法: 采用Phenomenex C₁₈色谱柱(4.6 mm×250 mm,5 μm),以乙腈(A)-0.3%磷酸溶液(B)为流动相,梯度洗脱(0~5 min,5%A→7%A;5~26 min,7%A;26~45 min,7%A→20%A;45~55 min,20%A→60%A;55~65 min,60%A),流速1 mL·min^-1,柱温40 ℃,波长切换(0~45 min,在240 nm波长下检测莫诺苷、芒果苷和马钱苷;46~65 min,在274 nm波长下检测丹皮酚). 结果: 莫诺苷、芒果苷、马钱苷和丹皮酚的线性范围分别为0.055 5~1.11 μg(r=0.999 9)、0.040 2~0.804 μg(r=0.999 9)、0.076 4~1.528 μg(r=0.999 9)、0.098 2~1.964 μg(r=0.999 9);平均回收率(n=6)分别为103.9%、102.0%、101.5%、102.2%,RSD分别为1.3%、1.3%、1.6%、0.82%.含量测定结果分别为1.117~1.501、0.375~0.447、1.083~1.562、2.306~2.857 mg·g^-1. 结论: 该方法操作稳定准确,重复性好,可用于知柏地黄丸(浓缩丸)的质量控制.

Objective: To develop an HPLC method for simultaneously determining 4 components including morroniside,chimonin,loganin and paeonol in Zhibai Dihuang pill(concentrated pill). Methods: The Phenomenex C₁₈ column(4.6 mm×250 mm,5 μm)was adopted.The mobile phase was acetonitrile(A)-0.3% aqueous phosphoric acid(B)by a gradient eluted program(0-15 min,5%A→7%A; 5-26 min,7%A; 26-45 min,7%A→20%A; 45-55 min,20%A→60%A; 55-65 min,60%A)with a flow rate of 1 mL·min^-1.The column temperature was 40 ℃.The detection wavelength was set at 240 nm for morroniside,chimonin and loganin in the first 45 min,and then changed to 274 nm for paeonol between 46 and 65 min. Results: The linear ranges of morroniside,chimonin,loganin and paeonol fell within the ranges of 0.055 5-1.11 μg(r=0.999 9),0.040 2-0.804 μg(r=0.999 9),0.076 4-1.528 μg(r=0.999 9),0.098 2-1.964 μg(r=0.999 9),respectively.The recoveries(n=6)of morroniside,chimonin,loganin and paeonol were 103.9%,102.0%,101.5%,102.2%,respectively,and the relative standard deviations were 1.3%,1.3%,1.6%,0.82%,respectively.The results of content assay were 1.117-1.501,0.375-0.447,1.083-1.562,2.306-2.857 mg·g^-1. Conclusion: This method is stable,accurate,reproducible and convenient for the quality control of Zhibai Dihuang pills(concentrated pills).

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