摘要
目的:建立一种可同时测定人参归脾丸和人参健脾丸中非法添加西洋参的超高效液相色谱串联质谱法(UPLC-MS/MS)检测方法。方法:用80%甲醇回流提取制备供试品溶液,使用Waters ACQUITY UPLC HSS T3 C_(18)色谱柱(100 mm×2.1 mm,1.8μm),乙腈-水为流动相进行梯度洗脱,流速为0.35 mL·min^(-1),柱温为40℃,采用电喷雾离子源、多反应监测模式、负离子方式进行扫描。结果:拟人参皂苷F_(11)在5.025~100.500 ng·mL^(-1)线性关系良好(r=0.9985),重复性RSD为1.4%,拟人参皂苷F_(11)在人参归脾丸和人参健脾丸中的回收率分别为97.71%、97.64%,检出限为1 ng·mL^(-1),定量限为3 ng·mL^(-1)。结论:建立的方法灵敏度高、实用性强,可作为人参归脾丸和人参健脾丸中非法投入西洋参的补充检验方法。
Objective:To establish a UPLC-MS/MS method for simultaneous determination of Panax quinquefolium illegally added in Renshen Jianpi Pills and Renshen Guipi Pills.Methods:The chromatographic separation was performed on Waters ACQUITY UPLC HSS T3 C_(18)(100 mm×2.1 mm,1.8μm)with acetonitrile and water as the mobile phases for gradient elution at a flow rate of 0.35 mL·min^(-1).The column temperature was 40℃,and the scanning was performed using electrospray ionization(ESI)source in multiple reaction monitoring(MRM)mode and negative ion mode.Results:Pseudo-ginsenoside F_(11) showed a good linearity in the concentration range of 5.025-100.500 ng·mL^(-1)(r=0.9985),and the relative standard deviation(RSD)of the repeatability test was 1.4%.The average recovery of pseudo-ginsenoside F_(11) was 97.71%in Renshen Guipi Pills and 97.64%in Renshen Jianpi Pills.The detection limit and the quantification limit was 1 ng·mL^(-1)and 3 ng·mL^(-1),respectively.Conclusion:The established method was highly sensitive and practical,and could be used as a supplementary test method for the illegal input of P.quinquefolium in Renshen Guipi Pills and Renshen Jianpi Pills.
作者
姚宝林
王然然
张淼
韦晶晶
尹贻珍
韩慧琴
YAO Bao-lin;WANG Ran-ran;ZHANG Miao;WEI Jing-jing;YIN Yi-zhen;HAN Hui-qin(Chengde City Institute for Food and Drug Control,Chengde 067000,China;Shijiazhuang Institute for Food and Drug Control,Shijiazhuang 050011,China;Zhangjiakou City Institute for Food and Drug Control,Zhangjiakou 075000,China)
出处
《中国现代中药》
CAS
2023年第1期150-156,共7页
Modern Chinese Medicine
基金
张家口市重点研发计划项目(2121037D)。
作者简介
通信作者:韩慧琴,副主任中药师,研究方向:中药质量标准,E-mail:2205006550@qq.com。
