高效液相色谱法同时检测枳实及枳壳药材中12种黄酮苷类成分  

Simultaneous Detection of 12 Flavonoid Glycosides in Aurantii Fructus Immaturus and Aurantii Fructus by HPLC

作　　者：曾辉 黄玉兰 税丕容 吕谦 ZENG Hui;HUANG Yulan;SHUI Pirong;LYU Qian(Luzhou Market Inspection and Testing Center,Luzhou,Sichuan,China 646000)

机构地区：[1]四川省泸州市市场检验检测中心,四川泸州646000

出　　处：《中国药业》2024年第2期75-79,共5页China Pharmaceuticals

基　　金：四川省药品监督管理局科技计划项目[2021007]。

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,5μm),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10μL。结果上述成分质量浓度分别在0.19~46.61μg/mL、0.17~43.27μg/mL、0.20~51.07μg/mL、11.34~756.01μg/mL、0.41~101.28μg/mL、20.58~1028.79μg/mL、0.20~50.49μg/mL、0.10~25.25μg/mL、0.10~26.63μg/mL、0.24~11.96μg/mL、0.21~52.64μg/mL、0.55~27.51μg/mL范围内与峰面积线性关系良好;检测限均不大于0.10μg/mL,定量限均不大于0.41μg/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。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-C_(18) column(250 mm×4.6 mm,5μm),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 10μL.Results The linear ranges of the above components were 0.19-46.61μg/mL,0.17-43.27μg/mL,0.20-51.07μg/mL,11.34-756.01μg/mL,0.41-101.28μg/mL,20.58-1028.79μg/mL,0.20-50.49μg/mL,0.10-25.25μg/mL,0.10-26.63μg/mL,0.24-11.96μg/mL,0.21-52.64μg/mL,0.55-27.51μg/mL,respectively.The limit of detection(LOD)was not greater than 0.10μg/mL,and the limit of quantification(LOQ)was not greater than 0.41μg/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.

关 键 词：高效液相色谱法 枳实 枳壳 黄酮苷 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]