UPLC波长切换法同时测定山茱萸中7个成分的含量

Simultaneous Determination of Seven Constituents in Corni Fructus by UPLC with Wavelength Switching

目的:建立UPLC波长切换法同时测定山茱萸中没食子酸、齐墩果酸、熊果酸、莫诺苷、当药苷、马钱苷和山茱萸新苷的含量。方法:采用Waters Acquituplc BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,以乙腈-0.3%磷酸溶液为流动相,梯度洗脱,流速0.5 ml·min-1,检测波长为273 nm(没食子酸)、240 nm(当药苷、马钱苷、山茱萸新苷)、360 nm(齐墩果酸、熊果酸),柱温30℃,进样量2μl。结果:没食子酸、齐墩果酸、熊果酸、莫诺苷、当药苷、马钱苷和山茱萸新苷检测质量浓度的线性范围分别为3.484~48.771,7.514~105.191,3.078~43.087,26.687~373.623,1.497~20.953,16.816~235.424,2.669~37.366μg·ml^-1(r为0.9993~0.9999);平均加样回收率分别为99.4%,100.4%,98.8%,99.5%,101.5%,100.2%,100.1%(RSD<2.0%,n=6);精密度、重复性、稳定性(24 h)试验的RSD<2.0%(n=6)。结论:该方法简单、有效、结果准确,可用于山茱萸中7个成分含量的同时测定。

Objective:To develop a method for the simultaneous determination of callic acid,oleanolic acid,ursolic acid,morroniside,sweroside,loganin and cornuside in Corni fructus by UPLC with wavelength switching.Methods:The analysis was carried out on a Waters Acquituplc BEH C18 column(2.1 mm×100 mm,1.7μm)with the mobile phase consisting of acetonitrile-0.3%phosphoric acid in a gradient mode at a flow rate of 0.5 ml·min-1.The detection wavelength was set at 273 nm for callic acid,240 nm for morroniside,sweroside,loganin and cornuside,and 360 nm for oleanolic acid and ursolic acid.The column temperature was set at 30℃and the injection volume was 2μl.Results:The linear range was 3.484-48.771,7.514-105.191,3.078-43.087,26.687-373.623,1.497-20.953,16.816-235.424 and 2.669-37.366μg·ml^-1 for callic acid,oleanolic acid,ursolic acid,morroniside,sweroside,loganin and cornuside,respectively(r=0.9993-0.9999).The average recovery was 99.4%,100.4%,98.8%,99.5%,101.5%,100.2%and 100.1%(RSD<2.0%,n=6),respectively.The RSDs of precision,reproducibility and stability tests(24 h)were all lower than 2.0%(n=6).Conclusion:The method is simple,effective and accurate,which can be used for the simultaneous determination of seven active constituents in Corni fructus.