UPLC-MS/MS检测乌鸡白凤丸中非法添加西洋参

Determination of Panax Quinquefolium Illegally Added in Wuji Baifeng Pills by UPLC-MS/MS

目的建立UPLC-MS/MS测定乌鸡白凤丸中非法添加的西洋参。方法使用Waters ACQUITY BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以乙腈和水为流动相,梯度洗脱,流速为0.35 mL·min^-1,柱温40℃,电喷雾电离源(ESI-),多反应离子监测(MRM)扫描方式进行检测。结果拟人参皂苷F11在0.113 0~451.9 ng·mL^-1范围内线性关系良好(r=0.999),重复性的相对标准偏差为3.5%,拟人参皂苷F11平均加样回收率(n=9)为96.9%,检出限为0.1ng·mL^-1,定量限为0.4 ng·mL^-1。结论所建立的方法快速准确、灵敏度高,可用于乌鸡白凤丸中非法添加西洋参的筛选和检测。

OBJECTIVE To establish adetection method for Panax quinquefolium a illegally added in Wuji Baifeng pills by UPLC-MS/MS. METHODS The analysis was performed on Waters ACQUITY BEH C18 column(2.1 mm×100 mm, 1.7 μm), with acetonitrile-water as the mobile phase with gradient elution and the flow rate of 0.35 mL·min-1. The column temperature was 40 ℃. The analytes were detected by tandem mass spectrometry with the electrospray ionization(ESI-) source combined with multiple reaction monitoring(MRM) mode. RESULTS Psuedo-ginsenoside F11 showed good linear relationship within the ranges of 0.113 0-451.9 ng·mL^-1(r=0.999), and the RSD of repeatability test was 3.5%. The average recovery(n=9) of pseudo-ginsenoside F11 was 96.9%. The limit of detection was 0.1 ng·mL^-1 and the limit of quantitation was 0.4 ng·mL^-1. CONCLUSION The established method is fast and accurate with a high sensitivity and a high degree of separation. It can be used for the screening and detection of Panax quinquefolium illegally added in Wuji Baifeng pills.