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

关键词:  超高效液相色谱-串联质谱法  乌鸡白凤丸  西洋参  拟人参皂苷F₁₁  非法添加

Key words:  UPLC-MS/MS  Wuji Baifeng pills  Panax quinquefolium  pseudo-ginsenoside F₁₁  illegally added

摘要:

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，1.7 μm），以乙腈和水为流动相，梯度洗脱，流速为0.35mL·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0.1130~451.9 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0.1 ng·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。

Abstract:

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.