首页|一测多评法同时测定一枝黄花中9个有效成分含量

一测多评法同时测定一枝黄花中9个有效成分含量

扫码查看
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,1.8 µm)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1 μL.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≥0.999 5);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.
Simultaneous determination of nine effective components in Solidaginis Herba by QAMS
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-ruti-noside,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,1.8 μm)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 1 μL.Chlorogenic acid and rutoside were chosen as the internal standards for phenolic acids and flavonoids respectively to establish the determine cor-rection factors of neochlorogenic acid,cryptochlorogenic acid,3,4-O-dicaffeoylquinic acid,3,5-O-dicaf-feoylquinic 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 ≥0.999 5),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.

Solidaginis Herbaphenolic acidsflavonoidschlorogenic acidcaffeoylquinic acidsrutosideiso-quercitrinkaemperol-3-O-rutinosidecontent determinationUPLCQAMS

杨群、肖文涛、刘德鸿

展开 >

九江市检验检测认证中心,九江 332000

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

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

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(7)
  • 20