论文部分内容阅读
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,5μm),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;5~26min,7%A;26~45 min,7%A→20%A;45~55 min,20%A→60%A;55~65 min,60%A),流速1 m L·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 5~1.11μg(r=0.999 9)、0.040 2~0.804μg(r=0.999 9)、0.076 4~1.528μg(r=0.999 9)、0.098 2~1.964μg(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 establish an HPLC method for simultaneous determination of morroniside, mangiferin, loganin and paeonol in Zhibai Dihuang Wan (Pill). Methods: The mobile phase was eluted with Phenomenex C18 column (4.6 mm × 250 mm, 5 μm) and acetonitrile (A) -0.3% phosphoric acid solution (B) for 0-5 min, 5% A → 7% A ; 5 to 26 min, 7% A; 26 to 45 min, 7% A to 20% A; 45 to 55 min, 20% A to 60% A; 55 to 65 min, 60% min-1, column temperature 40 ℃, wavelength switching (0 ~ 45 min, at 240 nm wavelength detection of morroniside, mangiferin and loganin; 46 ~ 65 min, the detection of paeonol at 274 nm wavelength). Results: The linear ranges of morroniside, mangiferin, loganin and paeonol were 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) and 0.098 2 ~ 1.964 μg (r = 0.999 9) respectively. The average recoveries were 103.9%, 102.0%, 101.5% and 102.2% respectively with RSDs of 1.3%, 1.3% 1.6%, 0.82%. The results of determination were 1.117-1.501,0.375-0.447,1.083-1.562 and 2.306-2.857 mg · g-1, respectively. Conclusion: The method is stable and accurate in operation with good reproducibility and can be used for quality control of Zhibai Dihuang Wan (Pills).