HPLC法同时测定前列癃闭通片中6个有效成分的含量  

Determination of six active ingredients in Qianlielong Bitong tablets by HPLC

作　　者：崔璐[1] 孙小玲 郝延军 潘延宁 陈婧 康廷国[1] 

机构地区：[1]辽宁中医药大学,大连116600 [2]辽宁省药品检验检测院,沈阳110023 [3]朝阳市食品药品检验所,朝阳122000

出　　处：《药物分析杂志》2015年第11期1914-1918,共5页Chinese Journal of Pharmaceutical Analysis

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.

关 键 词：前列癃闭通片 虎杖苷 柚皮苷 橙皮苷 新橙皮苷 朝藿定C 淫羊藿苷 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]