摘要
目的采用超高效液相-串联三重四级杆质谱(UPLC-MS/MS)法同时测定枳壳中14种黄酮类成分的含量,为中药材枳壳的质量评价提供参考。方法以甲醇作为提取溶剂,采用ACQUITY UPLC^(TM)BEH C_(18)(100 mm×2.1 mm,1.8μm)色谱柱,以0.1%甲酸乙腈(A)-0.1%甲酸水(B)为流动相,流速为0.6 mL·min^(-1);进样量为1.0μL,柱温为40℃。离子化模式为ESI+和ESI-,多反应监测模式(MRM)。利用外标法计算枳壳样品中黄酮类成分的含量,并结合化学计量学方法分析不同来源枳壳样品的差异。结果14种黄酮类成分在考察浓度范围内,浓度与峰面积之间线性关系良好(r^(2)>0.999);精密度、重复性和稳定性实验考察结果良好;橙皮素、柚皮素、橙皮苷、芦丁、异牡荆苷、忍冬苷、异鼠李素3-O-葡萄糖苷、圣草次苷、芸香柚皮苷、川陈皮素、枸橘苷、桔皮素、柚皮苷、新橙皮苷的平均回收率(n=6)范围在98.8%~102.1%之间,其RSD值均小于5%。主成分分析结果显示橙皮素、柚皮素、异鼠李素3-O-葡萄糖苷、川陈皮素、枸橘苷和桔皮素6个成分可有效区分酸橙、代代花、臭橙以及香橙4种不同来源枳壳。结论该方法准确、重复性好、检测限低,可客观反映出不同来源枳壳的差异,为进一步完善枳壳质量研究提供参考依据。
Objective To establish a UPLC-MS/MS method for the simultaneous determination of 14 flavonoids in Fructus Aurantii,providing a reference for the quality evaluation of Fructus Aurantii.Methods Use methanol as extraction solvent,and the ACQUITY UPLC^(TM)BEH C_(18)(100 mm×2.1 mm,1.8μm)column was used.Acetonitrile-0.1%formic acid and water containing 0.1%formic acid were used as the mobile phase and eluted at a flow rate gradient of 0.6 mL·min^(-1).The column temperature was 40℃.The components were detected in multiple reaction monitoring modes by mass spectrometry with ionization mode of ESI+and ESI-.The content of the components measured in the samples was calculated by using the external standard method,and combining chemometric methods to analyze the differences between the samples of Fructus Aurantii from different origins.Results Within the concentration range of the investigation of the 14 kinds of flavonoids,the linear relationship between concentration and peak area is good(r^(2)>0.999);The precision experiment,repeatability experiment,and stability experiment are all good.The mean recovery rate of Hesperetin,,Naringenin,hesperidin,Rutin,Isovitexin,Lonicerin,Isorhamnetin 3-O-glucoside,Eriocitrin,,Narirutin,Nobiletin,Poncirin,Tangeretin,Naringin,and Neohesperidin(n=6)ranges from 98.8%to 102.1%.The RSD values are all less than 5%.The principal component analysis showed that the 6 components of Hesperetin,Naringenin,Isorhamnetin 3-O-glucoside,Nobiletin,Poncirin,and Tangeretin can effectively distinguish 4 kind origins of Fructus Aurantii,C.aurantium L.,C.aurantium′Daidai′,C.aurantium cv.Xiucheng,and C.junos Siebold ex Tanaka.Conclusion The method is accurate results,good repeatability,a low detection limit,and can objectively reflect the differences in the content of main flavonoids of Fructus Aurantii from different origins.It provides a reference for further improving the quality research of Fructus Aurantii.
作者
陈慧轩
李翔
杨健
张小波
Chen Huixuan;Li Xiang;Yang Jian;Zhang Xiaobo(School of Pharmacy,Jangsu University,Zhenjiang 212013,China;State Key Laboratory of Daodi Herbs,National Resource Center for Chinese Materia Medical Sciences,Beijing 100700,China;Jiangxi Provincial Quality Evaluation and Research Center for Authentic Medicinal Materials,Nanchang 330000,China)
出处
《世界科学技术-中医药现代化》
CSCD
北大核心
2023年第2期519-526,共8页
Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology
基金
中国中医科学院科技创新工程重大攻关项目(CI2021A03901):全国中药材生产统计规范编研及示范应用,负责人:张小波
中国中医科学院中央本级重大增减支项目(2060302):中药资源普查和药用植物识别数据库保障条件建设,负责人:张小波
国家中医药管理局中医药创新团队及人才支持计划项目(ZYYCXTD-D-202005):中药资源普查成果价值挖掘与转化应用,负责人:张小波
