一测多评法同时测定一枝黄花中9个有效成分含量  

Simultaneous determination of nine effective components in Solidaginis Herba by QAMS

作　　者：杨群 肖文涛 刘德鸿 YANG Qun;XIAO Wen-tao;LIU De-hong(Jiujiang Inspection,Testing and Certification Center,Jiujiang 332000,China;Jiangxi Institute for Drug Control,National Medical Products Administration Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Engineering Research Center for Drug and Medical Device Quality,Nanchang 330029,China)

机构地区：[1]九江市检验检测认证中心,九江332000 [2]江西省药品检验检测研究院、国家药品监督管理局中成药质量评价重点实验室江西省药品与医疗器械质量工程技术研究中心,南昌330029

出　　处：《药物分析杂志》2024年第7期1186-1194,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立一测多评法同时测定一枝黄花中酚酸类及黄酮类共9个成分(新绿原酸、绿原酸、隐绿原酸、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、3,4-O-二咖啡酰奎宁酸、3,5-O-二咖啡酰奎宁酸和4,5-O-二咖啡酰奎宁酸)的含量。方法:采用超高效液相色谱法,采用ACQUITY UPLC®HSS T3(100 mm×2.1 mm,1.8μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(B)为流动相进行梯度洗脱,流速0.3 mL·min^(-1),检测波长327 nm,柱温30℃,进样量1μL。酚酸类成分以绿原酸为内标,黄酮类成分以芦丁为内标,采用多点校正法,分别建立新绿原酸、隐绿原酸、3,4-O-二咖啡酰奎宁酸、3,5-O-二咖啡酰奎宁酸、4,5-O-二咖啡酰奎宁酸和异槲皮苷、山柰酚-3-O-芸香糖苷的相对校正因子,并计算其含量。测定结果与外标法结果进行比较,验证其准确性。结果:9个成分在各自范围内线性关系良好(r≥0.9995);平均加样回收率分别为98.2%~101.7%,RSD分别为1.0%~1.7%。9批样品中新绿原酸、绿原酸、隐绿原酸、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、3,4-O-二咖啡酰奎宁酸、3,5-O-二咖啡酰奎宁酸和4,5-O-二咖啡酰奎宁酸的含量范围分别为0.008%~0.014%、0.055%~0.097%、0.010%~0.019%、0.191%~0.412%、0.018%~0.035%、0.116%~0.250%、0.028%~0.048%、0.111%~0.235%、0.113%~0.182%。一测多评法测定结果与外标法结果一致(相对平均偏差<2.8%)。结论:该方法简便、准确,重复性好,可用于一枝黄花药材的质量控制。Objective:To establish a quantitative analysis of multi-components by single marker(QAMS)method for the simultaneous determination of nine effective components including phenolic acids and flavonoids(neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,rutoside,isoquercitrin,kaemperol-3-O-rutinoside,3,4-O-dicaffeoylquinic acid,3,5-O-dicaffeoylquinic acid,4,5-O-dicaffeoylquinic acid),in Solidaginis Herba.Methods:Ultra-high performance liquid chromatography was developed on an ACQUITY UPLC®HSS T3(100 mm×2.1 mm,1.8μm)column with acetonitrile(A)-0.1%phosphoric acid solution(B)as mobile phase in gradient elution.The flow rate was 0.3 mL·min^(-1),the detection wavelength was 327 nm,the column temperature was 30℃,and the injection volume was 1μL.Chlorogenic acid and rutoside were chosen as the internal standards for phenolic acids and flavonoids respectively to establish the determine correction factors of neochlorogenic acid,cryptochlorogenic acid,3,4-O-dicaffeoylquinic acid,3,5-O-dicaffeoylquinic acid,4,5-O-dicaffeoylquinic acid isoquercitrin and kaemperol-3-O-rutinoside,respectively,by multi-point correction method and their contents were calculated.The results were compared with the results of external standard method to verify their accuracy.Results:Nine components showed good linear relationships within their own ranges(r≥0.9995),whose average recoveries were 98.2%-101.7%with the RSDs of 1.0%-1.7%.The contents of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,rutoside,isoquercitrin,kaemperol-3-O-rutinoside,3,4-O-dicaffeoylquinic acid,3,5-O-dicaffeoylquinic acid and 4,5-O-dicaffeoylquinic acid,in nine batches of samples were 0.008%-0.014%,0.055%-0.097%,0.010%-0.019%,0.191%-0.412%,0.018%-0.035%,0.116%-0.50%,0.028%-0.048%,0.111%-0.235%and 0.113%-0.182%.The results obtained by QAMS were consistent with those of external standard method(relative average deviations less than 2.8%).Conclusion:The simple,accurate and reproducible method can be used for the quality control of Solidaginis Herba.

关 键 词：一枝黄花 酚酸 黄酮 绿原酸 咖啡酰奎宁酸 芦丁 异槲皮苷 山柰酚-3-O-芸香糖苷 含量测定 超高效液相色谱 一测多评 

分 类 号：R917[医药卫生—药物分析学]