HPLC法同时测定前列癃闭通片中6个有效成分的含量

目的:建立同时测定前列癃闭通片中虎杖苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷含量的HPLC法。方法:采用SHISEIDO-C₁₈色谱柱(4.6 mm×200 mm,5μm),流动相为乙腈(A)-水(B),采用梯度洗脱(0~10 min,18%A;10~35 min,18%A→25%A;35~38 min,25%A→28%A;38~55 min,28%A;55~60 min,28%A→18%A),流速1.0 mL·min^-1,柱温35℃,检测波长为306 nm(0~15 min,测定虎杖苷)、283 nm(15~35 min,测定柚皮苷、橙皮苷、新橙皮苷)、270 nm(35~60 min,测定朝藿定C、淫羊藿苷)。结果:虎杖苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C和淫羊藿苷进样量分别在0.0202~0.2016 μg(r=0.9996)、0.0992~0.9924 μg(r=0.9997)、0.0309~0.3092 μg(r=0.9997)、0.0892~0.8924 μg(r=0.9997)、0.0369~0.3686 μg(r=0.9999)和0.1045~1.0451 μg(r=0.9999)范围内线性关系良好;平均加样回收率(n=6)分别为99.7%、101.2%、101.4%、99.8%、98.7%和97.9%,RSD分别为0.95%、1.2%、1.0%、0.97%、1.3%和1.1%。4批样品6个活性成分的含量测定结果为虎杖苷0.643~0.652 mg·g^-1,柚皮苷2.293~2.325 mg·g^-1,橙皮苷0.700~0.715 mg·g^-1,新橙皮苷1.878~1.900 mg·g^-1,朝藿定C 0.735~0.747 mg·g^-1,淫羊藿苷2.042~2.050 mg·g^-1。结论:该方法操作简单,重复性好,可作为评价和监控前列癃闭通片质量的方法。

Objective: To establish a method for simultaneous determination of six active ingredients (polydatin, naringin, hesperidin, neohesperidin, epimedin C, icariin) in Qianlielong Bitong tablets. Methods:The determination was carried out with a SHISEIDO-C₁₈ column (4.6 mm×200 mm,5μm). The mobile phase consisted of acetonitrile (A)-water(B) with gradient elution (0-10 min, 18%A; 10-35 min, 18%A→25%A; 35-38 min, 25%A→28%A; 38-55 min,28%A; 55-60 min, 28%A→18%A) at a flow rate of 1.0 mL·min^-1. The column temperature was set at 35℃. The detection wavelengths were 306 nm in 0-15 min for polydatin, 283 nm in 15-35 min for naringin, hesperidin and neohesperidin, and 270 nm in 35-60 min for epimedin C and icariin. Results: The calibration curves were linear within the range of 0.020 2-0.201 6 μg for polydatin (r=0.999 6), 0.099 2-0.992 4 μg for naringin (r=0.999 7), 0.030 9-0.309 2 μg for hesperidin (r=0.999 7), 0.089 2-0.892 4 μg for neohesperidin (r=0.999 7), 0.036 9-0.368 6 μg for epimedin C (r=0.999 9), 0.104 5-1.045 1 μg for icariin (r=0.999 9). The average recoveries (n=6) were 99.7%, 101.2%, 101.4%, 99.8%, 98.7% and 97.9%; RSDs were 0.95%, 1.2%, 1.0%, 0.97%, 1.3% and 1.1%, respectively. The contents of the six active ingredients in 4 samples were in the range of 0.643-0.652 mg·g^-1 for polydatin, 2.293-2.325 mg·g^-1 for naringin, 0.700-0.715 mg·g^-1 for hesperidin, 1.878-1.900 mg·g^-1 for neohesperidin, 0.735-0.747 mg·g^-1 for epimedin C, and 2.042-2.050 mg·g^-1 for icariin. Conclusion:The method is simple to operate and has good repeatability, and thus can be applied to the evaluation and quality control of Qianlielong Bitong tablets.