HPLC-PDA检测补肾中成药中十一种PDE5型抑制剂

HPLC-PDA detection of eleven PDE5 inhibitors in kidney-tonifying Chinese patent medicines

目的:建立HPLC-PDA筛查补肾中成药中十一种PDE5型抑制剂的方法。方法:Eclipe XDB-C18 (4.6×250mm,5 μm)色谱柱,流动相A为乙腈,流动相B为含0.1%醋酸的5 mmol/L醋酸铵水溶液,流速1.0 mL/min,柱温30℃,检测波长290 nm,梯度洗脱并采集200~400 nm范围的吸收光谱。结果:十一种PDE5型抑制剂在100~1000 ng范围内,线性关系良好,r均大于0.9999,平均回收率为93.09%~108.45%,相对标准偏差为0.64%~1.06%,检测限为0.23~1.03 ng。结论:该方法稳定、灵敏度高、简单易掌握,适合基层市场监督机构监测大批量补肾中成药中非法添加的十一种PDE5型抑制剂。

Objective:To establish a HPLC-PDA method for screening eleven PDE5 inhibitors in kidney-tonifying Chinese patent medicines.Method:Eclipe XDB-C18(4.6×250 mm,5μm) chromatographic column was used to analyze.Mobile phase A was acetonitrile,mobile phase B was 5 mmol·L-1 ammonium acetate aqueous solution containing 0.1% acetic acid.The flow rate was 1.0 mL·min^(-1).Column temperature was 30℃.The detection wavelength was 290 nm.Gradient elution was performed and the absorption spectrum in the range of 200~400 nm was collected.Result:The eleven PDE5 inhibitors had a good linear relationship in the range of 100~1000 ng,with r all greater than 0.9999.The average recovery was 93.09%~108.45%,and the relative standard deviation was 0.64%~1.06%.The detection limit was 0.23~1.03 ng.Conclusion:This method is stable,highly sensitive,simple and easy to master,and is suitable for the monitoring of eleven PDE5 inhibitors illegally added in large quantities of kidneytonifying Chinese patent medicines by the primary market supervision agency.