摘要
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 m L·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0.020 2~0.201 6μg（r=0.999 6）、0.099 2~0.992 4μg（r=0.999 7）、0.030 9~0.309 2μg（r=0.999 7）、0.089 2~0.892 4μg（r=0.999 7）、0.036 9~0.368 6μg（r=0.999 9）和0.104 5~1.045 1μg（r=0.999 9）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, ieariin） in Qianlielong Bitong tablets. Methods ：The determination was carried out with a SH1SEIDO-C18 column （4.6 mm × 200 mm,5 μm）. 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 rain, 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 rain for epimedin C and ieariin. 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 ieariin （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 neohesper/din, 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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第11期1914-1918,共5页
Chinese Journal of Pharmaceutical Analysis
