摘要
目的建立HPLC波长切换联合梯度洗脱法同时测定藿香鼻炎合剂中的广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素含量的方法。方法采用Kromasil C_(18)(4.6 mm×250 mm,5μm)色谱柱;流动相A:乙腈,流动相B:0.4%磷酸溶液,进行梯度洗脱;流速:1.0 mL/min;柱温:30℃;检测波长分别规定为310 nm(广藿香酮)、280 nm(黄芩苷、汉黄芩苷、黄芩素和汉黄芩素)。结果广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素的线性范围分别为4.300~86.00μg/mL(r=0.999 6)、15.87~317.4μg/mL(r=0.999 8)、6.920~138.4μg/mL(r=0.9999)、6.340~126.8μg/mL(r=0.999 4)、5.250~105.0μg/mL(r=0.999 8),平均加样回收率和RSD均符合中国药典规定。结论本文建立的HPLC波长切换联合梯度洗脱法同时测定广藿香酮、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素5个成分,方法专属性强,重复性好,可作为藿香鼻炎合剂全面可靠的质量控制方法。
Objective To develop a method of wavelength switching HPLC combined with gradient elution for determination of the content of pogostone,baicalin,wogonoside,baicalein and wogonin in Huoxiang Biyan Mixture.Methods A kromasil C_(18)(4. 6 mm × 250 mm,5 μm) column was used as the chromatographic column,the mobile phase was acetonitrile( A) and 0. 4% phosphoric acid solution( B),and gradient elution was performed;the flow rate was 1. 0 mL/min,and the column temperature was set at 30 ℃. Pogostone was detected at 310 nm; the baicalin,wogonoside,baicalein and wogonin were detected at 280 nm. Results Pogostone,baicalin,wogonoside,baicalein and wogonin had good linearities in 4. 300 ~ 86. 00 μg/mL( r = 0. 999 6),15. 87 ~ 317. 4 μg/mL( r = 0. 999 8),6. 920 ~138. 4 μg/mL( r = 0. 999 9),6. 340 ~ 126. 8 μg/mL( r = 0. 999 4) and 5. 250 ~ 105. 0 μg/mL( r = 0. 999 8),respectively. The average recovery and RSD all met the requirements of Pharmacopoeia of The People's Republic of China.Conclusion The method of wavelength switching HPLC combined with gradient elution has been successfully established for simultaneous determination of 5 components in Huoxiang Biyan Mixture. The method is safe and reproducible,and is helpful for the quality control of Huoxiang Biyan Mixture.
引文
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