RP-HPLC测定牛黄消炎片中华蟾酥毒基和脂蟾毒配基的含量

RP-HPLC determination of cinobufagin and resibufogenin in Niuhuangxiaoyan Tablet

目的 :建立牛黄消炎片 (牛黄、大黄、珍珠母、蟾酥等 )中华蟾酥毒基和脂蟾毒配基的高效液相含量测定方法。方法 :WatersSymmetryShieldRP1 8(3.9mm× 2 5 0mm ,5 μm) ,流动相为乙腈 0 .5mol·L-1 磷酸二氢钾溶液 (pH用磷酸调节值至3.2 ) (42∶5 8) ;柱温 30℃ ;流速 1 .0mL·min-1 ,检测波长为 2 96nm。结果 :华蟾酥毒基线性范围为 0 .0 6 96～ 0 .835 2 μg ,精密度试验RSD为 0 .72 %,稳定性试验RSD为 0 .5 6 %,重现性试验RSD为 4 .2 8%,回收率为 1 0 0 .0 6 %,RSD为 1 .2 5 %;脂蟾毒配基线性范围为 0 .1 5 76～ 0 .94 5 6 μg ,精密度试验RSD为 0 .4 3%,稳定性试验RSD为 0 .84 %,重现性试验RSD为 4 .35 %,回收率为 1 0 0 .5 4 %,RSD为 1 .4 9%。结论 :本方法快速、准确、重现性较好 ,结果可靠 ,为牛黄消炎片提供有效的质量评价方法。

AIM: To estalish a HPLC method for the determination of cinobufagin and resibufogenin in Niuhuangxiaoyan Tablet(Calculus Bovls, Radix et Rhizoma Rhei, Concha Margaritifera Usta, Venenum Bufonis, etc.). METHODS: Waters Symmetry Shield RP18(3.9mm×250mm,5μm) column at 30℃ was used with a mobile phase consisted of acetonitrile -0.5mol·L -1 potassium dihydrogen phosphate(solution was adjusted by phosphoric acid to pH=3.2) (42∶58) and a UV detector at 296nm. The flow rate was 1.0mL·min -1 . RESULTS: The linear range of cinobufagin was 0.0696～0.8352μg. The RSD of measurement precision test was 0.53%; The average recovery was 100.06% ( RSD =1.25%, n =5). The linear range of resibufogenin was 0.1576～0.9456μg. The RSD of measurement precision test was 0.15%. The average recovery was 100.54%( RSD =1.49%, n =5). CONCLUSION: The method is simple and accurate, and can be used for the quality control of Niuhuangxiaoyan Tablet.