摘要
目的 建立同时检测枳实、枳壳药材中 12 种黄酮苷类成分的高效液相色谱法.方法 色谱柱为Agilent Zorbax SB-C18 柱(250 mm×4.6 mm,5 μm),流动相为 0.1%甲酸水溶液-乙腈(梯度洗脱),流速为 1.0 mL/min,检测波长为 284 nm(圣草次苷、新北美圣草苷、芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、枸橘苷、柚皮素、橙皮素)、330 nm(橙皮内酯、川陈皮素、橘红素),柱温为 35℃,进样量为 10 μL.结果 上述成分质量浓度分别在 0.19～46.61 μg/mL、0.17～43.27 μg/mL、0.20～51.07 μg/mL、11.34～756.01 μg/mL、0.41～101.28 μg/mL、20.58～1028.79 μg/mL、0.20～50.49 μg/mL、0.10～25.25 μg/mL、0.10～26.63 μg/mL、0.24～11.96 μg/mL、0.21～52.64 μg/mL、0.55～27.51 μg/mL范围内与峰面积线性关系良好;检测限均不大于0.10 μg/mL,定量限均不大于0.41 μg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为92.90%～114.33%,RSD为0.30%～1.98%(n=9).结论 所建立的方法简便、可靠,可用于同时检测枳实、枳壳药材中 12 种黄酮苷类成分.
Abstract
Objective To establish a high-performance liquid chromatography method for simultaneous detection of 12 flavonoid glycosides in Aurantii Fructus Immaturus and Aurantii Fructus.Methods The chromatographic column was Agilent Zorbax SB-C18 column(250 mm×4.6 mm,5 μm),the mobile phase was 0.1%formic acid aqueous solution-acetonitrile(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 284 nm(eriocitrin,neoeriocitrin,narirutin,naringin,hesperidin,neohesperidin,poncirin,naringenin,hesperetin),330 nm(meranzin,nobiletin,tangeretin),the column temperature was 35℃,and the injection volume was 10 μL.Results The linear ranges of the above components were 0.19-46.61 μg/mL,0.17-43.27 μg/mL,0.20-51.07 μg/mL,11.34-756.01 μg/mL,0.41-101.28 μg/mL,20.58-1 028.79 μg/mL,0.20-50.49 μg/mL,0.10-25.25 μg/mL,0.10-26.63 μg/mL,0.24-11.96 μg/mL,0.21-52.64 μg/mL,0.55-27.51 μg/mL,respectively.The limit of detection(LOD)was not greater than 0.10 μg/mL,and the limit of quantification(LOQ)was not greater than 0.41 μg/mL.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of above components were in the range of 92.90%to 114.33%,with the RSDs of 0.30%to 1.98%(n = 9).Conclusion The established method is simple and reliable,which can be used for the simultaneous detection of 12 flavonoid glycosides in Aurantii Fructus Immaturus and Aurantii Fructus.
基金项目
四川省药品监督管理局科技计划项目(2021007)
国家科技期刊平台
NSTL
万方数据