摘要
目的建立一测多评法(QAMS)测定藏茴香中6种咖啡酰奎宁酸类成分含量,并验证该方法在藏茴香质量评价中应用的可行性与适用性。方法取藏茴香粉末(过三号筛)0.5 g,精密加入70%甲醇20 mL,超声处理(250 W、频率53 kHz)30 min,制备供试品溶液;采用Phenomenex GeminiR C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,检测波长为330 nm,体积流量1.0 mL·min^(−1),柱温30℃,进行专属性、供试品提取条件、检测波长选择、色谱条件、线性关系、精密度、重复性、稳定性、加样回收率方法学考察,建立异绿原酸A、新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸C成分含量检测的HPLC法;以异绿原酸A为内参成分,分别计算新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸C 5种成分的相对校正因子,分别采用3种不同色谱仪和3种色谱柱进行相对校正因子、相对保留时间耐用性考察,对藏茴香样品同时采用外标法与QAMS测定6种成分的质量分数,比较2种测定方法结果的差异。结果建立的6种成分的HPLC检测方法的专属性、供试品提取条件、检测波长选择、色谱条件、线性关系、精密度、重复性、稳定性、加样回收率均符合要求;新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸C的相对校正因子平均值分别是1.362、1.257、1.335、1.470、1.134,3种不同色谱仪和3种色谱柱对相对校正因子、相对保留时间均无明显影响;QAMS与外标法2种方法测定3批藏茴香样品中6种成分得到的结果之间无显著差异。结论建立的QAMS简便、准确、可靠,可用于藏茴香中6种咖啡酰奎宁酸类成分——异绿原酸A、新绿原酸、绿原酸、隐绿原酸、异绿原酸B、异绿原酸C的定量分析。
Objective To establish a method for the content determination of six caffeoylquinic acids components in Carum carvi L.through quantitative analysis of multi-components with single marker(QAMS).To verify the feasibility and applicability of the method in its quality control.Methods Take 0.5 g of C.carvi powder(through the third sieve),accurately add 20 mL of 70%methanol,and conduct ultrasonic treatment(250 W,frequency 53 kHz)for 30 min to prepare the test solution.Phenomenex GeminiR C_(18) column(250 mm×4.6 mm,5μm)was used,acetonitrile-0.1%formic acid aqueous solution was used as mobile phase,gradient elution,flow rate was 1.0 mL·min^(−1),column temperature was 30℃,and detection wavelength was 330 nm.Conduct methodological studies on specificity,test article extraction conditions,detection wavelength selection,chromatographic conditions,linear relationship,precision,repeatability,stability,and sample addition recovery.With isochlorogenic acid A as the internal reference component,relative correction factors of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,isochlorogenic acid B and isochlorogenic acid C was established.Three different chromatographs and three chromatographic columns were used to investigate the relative correction factor and relative retention time durability.The external standard method and QAMS were used to simultaneously determine the mass fractions of six components in C.carvi samples,and the differences between the two determination results were compared.Results The specificity,extraction conditions,detection wavelength selection,chromatographic conditions,linear relationship,precision,repeatability,stability,and sample recovery of the established HPLC detection methods for the six components meet the requirements.The relative positive factors of isochlorogenic acid A and neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,isochlorogenic acid B and isochlorogenic acid C were 1.362,1.257,1.335,1.470,and 1.134,respectively.Three different chromatographs and three chr
作者
周凡
李淑萍
贺飞
吴涛
阿吉艾克拜尔·艾萨
买吾兰江·买提努尔
ZHOU Fan;LI Shuping;HE Fei;WU Tao;Haji Akber Aisa;Maitinuer Maiwulanjiang(State Key Laboratory Basis of Xinjiang Indigenous Medicinal Plants Resource Utilization,CAS Key Laboratory of Chemistry of Plant Resources in Arid Regions,Xinjiang Technical Institute of Physics and Chemistry,Chinese Academy of Sciences,Urumqi 830011,China;University of Chinese Academy of Sciences,Beijing 100049,China)
出处
《药物评价研究》
CAS
2023年第4期703-710,共8页
Drug Evaluation Research
基金
新疆维吾尔自治区自然科学基金资助项目(2022D01E94)
新疆维吾尔自治区天山英才培养计划资助项目(2022TSYCCX0023)。
关键词
藏茴香
一测多评法
相对校正因子
咖啡酰奎宁酸
异绿原酸A
新绿原酸
绿原酸
隐绿原酸
异绿原酸B
异绿原酸C
Carum carvi L.
quantitative analysis of multi-components with single marker(QAMS)
relative correction factor
caffeoylquinic acids
isochlorogenic acid A
neochlorogenic acid
chlorogenic acid
cryptochlorogenic acid
isochlorogenic acid B
isochlorogenic acid C
