RP-HPLC法测定肾炎四味片中黄芩苷、木犀草素和山柰素的含量  

Determination of baicalin,luteolin and kaempferide in Shenyansiwei tablets by RP- HPLC

作　　者：王笑笑 方一超 周勇 徐宇昌 程巧鸳 颜伟华 

机构地区：[1]衢州市食品药品检验研究院,衢州324002 [2]衢州市市场监督管理局,衢州324002 [3]浙江省食品药品检验研究院,杭州310000

出　　处：《药物分析杂志》2015年第10期1857-1861,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立测定肾炎四味片中黄芩苷、木犀草素和山柰素含量的方法。方法：采用Eclipse XDB-C18色谱柱（250 mm×4.6 mm,5μm）,以甲醇（A）-0.2%磷酸水溶液（B）为流动相,梯度洗脱（0～20 min,40%A→60%A;20～25 min,60%A;25～29 min,60%A→90%A;29～32 min,90%A→40%A）,流速1.0 m L·min-1,检测波长为279 nm（0～17 min）和267 nm（17～25 min）,柱温25℃。结果：黄芩苷、木犀草素和山柰素的线性范围分别为0.039～7.800μg（r=0.999 9）、0.032～6.454μg（r=0.999 9）和0.001～0.288μg（r=0.999 9）;平均加样回收率（n=6）分别为98.09%、99.10%和99.73%,RSD分别为1.9%、2.3%和2.7%。3批样品的测定结果分别为每片含黄芩苷13.482、13.520、14.524 mg,木犀草素9.120、7.246、8.615 mg,山奈素0.278、0.219、0.294 mg。结论 ：所建立的方法经方法学验证,可作为肾炎四味片的质量控制方法。Objective： To develop an HPLC method for the content determination of baicalin,luteolin and kaempferide in Shenyansiwei tablets. Methods： The separation was performed on an Eclipse XDB- C18column（ 250 mm × 4. 6 mm,5 μm） with the mobile phase consisting of methanol（ A）-0. 2% phosphoric acid solution（ B）in gradient elution（ 0-20 min,40% A→60% A; 20-25 min,60% A; 25-29 min,60% A→90% A; 29-32 min,90%A→40% A）. The flow rate was 1. 0 m L·min- 1,the detection wavelength were 279 nm（ 0-17 min） and 267 nm（ 17-25 min）,and the temperature was controlled at 25 ℃. Results： The calibration curves were linear within the ranges of 0. 039-7. 800 μg（ r = 0. 999 9）,0. 032-6. 454 μg（ r = 0. 999 9） and 0. 001-0. 288 μg（ r = 0. 999 9） for baicalin,luteolin and kaempferide,respectively. The average recoveries were 98. 09%,99. 10% and 99. 73%,and the RSDs were 1. 9%,2. 3% and 2. 7%. The measurement results of three batches of samples were 13. 418 mg,13. 520 mg,and 14. 524 mg for baicalin,9. 120,7. 246,and 8. 615 mg for luteolin,0. 278,0. 219,and 0. 294 mg for kaempferide. Conclusion： The method is applicable for simultaneous determination of baicalin,luteolin and kaempferide in Shenyansiwei tablets by methodology validation.

关 键 词：肾炎四味片 细梗胡枝子 黄芩苷 木犀草素 山柰素 黄酮类成分 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]