摘要
目的:建立同时测定硫磺熏蒸前后当归中阿魏酸、藁本内酯、丁烯基苯酞、洋川芎内酯A、洋川芎内酯H、洋川芎内酯I、欧当归内酯A等7种活性成分含量的方法。方法:采用超高效液相色谱法。色谱柱为Waters BEH C18,流动相为1%醋酸-甲醇(梯度洗脱),柱温为30℃,流速为0.35m L/min,检测波长为254nm,进样量为2μL。结果:阿魏酸、藁本内酯、丁烯基苯酞、洋川芎内酯A、洋川芎内酯H、洋川芎内酯I、欧当归内酯A检测进样量的线性范围分别为0.021 6～0.324 0、0.327 2～4.908 0、0.011 51～0.172 7、0.055 0～0.825 0、0.002 248～0.033 72、0.007 2～0.108、0.001 08～0.016 2μg(r2=0.999 1～1.000 0);检测限分别为3.7、0.56、0.52、2.02、0.007 6、1.16、0.64ng;定量限分别为11.5、1.85、1.66、6.26、0.076、3.36、1.79ng;精密度、稳定性、重复性试验的RSD均<3.0%(n=6);7种成分平均加样回收率为95.79%～101.70%,RSD为2.10%～2.93%(n=6)。硫磺熏蒸后对当归中7种活性成分含量的影响较大,总体呈下降趋势。结论:本研究建立的方法的精密度、稳定性、重复性均较好,可用于硫磺熏蒸前后当归中7种活性成分的含量测定;硫磺熏蒸后会降低当归中活性成分的含量。
OBJECTIVE:To establish the method for content determination of 7 kinds of active components that as ferulic acid,ligustilide,n-butylidenephthalide,senkyunolide A,senkyunolide H,senkyunolide I and levistilide A in Angelica sinensis before and after sulfur fumigation simultaneously.METHODS:UPLC method was adopted.The determination was performed on Waters BEH C18 column with mobile phase consisted of 1%acetic acid-methanol(gradient elution)at flow rate of 0.35 mL/min.The column temperature was 30℃,and detection wavelength was set at 254 nm.The sample size was 2μL.RESULTS:The linear range for ferulic acid,ligustilide,n-butylidenephthalide,senkyunolide A,senkyunolide H,senkyunolide I and levistilide A was 0.021 6-0.324 0,0.327 2-4.908 0,0.011 51-0.172 7,0.055 0-0.825 0,0.002 248-0.033 72,0.007 2-0.108,0.001 08-0.016 2μg(r2=0.999 1-1.000 0),respectively.The limits of detection were 3.7,0.56,0.52,2.02,0.007 6,1.16,0.64 ng,respectively.The limits of quantitation were 11.5,1.85,1.66,6.26,0.076,3.36,1.79 ng,respectively.RSDs of precision,stability and reproducibility tests were lower than 3.0%(n=6).The average recovery rates of 7 kinds of active components were from 95.79%to 101.70%(RSD=2.10%-2.93%,n=6).The contents of active 7 kinds of active components in A.sinensis were greatly influenced by sulfur fumigation and had a downward trend in general.CONCLUSIONS:The established method is simple with good precision,stability and reproducibility and can be used for the content determination of 7 kinds of active components in A.sinensis before and after sulfur fumigation.The sulfur fumigation will decrease the contents of active components in A.sinensis.c
作者
史雪霞
李运
SHI Xuexia;LI Yun(Dept.of Pharmacy,the Affiliated Hospital of Qinghai University,Xining 810001,China;Lanzhou Institute for Food and Drug Control,Lanzhou 730000,China)
出处
《中国药房》
CAS
北大核心
2018年第17期2389-2393,共5页
China Pharmacy
基金
兰州市科技计划项目(No.2016-3-17)
作者简介
史雪霞:副主任药师。研究方向:医院药学。电话:0971-6162050。E-mail:515798280@qq.com
