Aim To determine calycosin-7-O-β-D-glucoside,astragaloside IV and formononetin in Radix Astragali and other relative samples by HPLC-MS.Methods HPLC was carried out with Agilent 1100LC/MSD,equipped with Agilent Zorba...Aim To determine calycosin-7-O-β-D-glucoside,astragaloside IV and formononetin in Radix Astragali and other relative samples by HPLC-MS.Methods HPLC was carried out with Agilent 1100LC/MSD,equipped with Agilent Zorbax SB C18 column（250 mm×4.6 mm ID,5 μm） and mass spectrum detector.The mobile phase（CH3CN-H2O） was eluted in gradient mode.Results The calibration curves of calycosin-7-O-β-D-glucoside,astragaloside IV and formononetin were linear in the range of 0.031.21 μg·mL-1,0.35-13.86 μg·mL-1 and 0.38-15.22 μg·mL-1,respectively.These recoveries of samples were from 95% to 105% with RSD less than 1.5%.Conclusion The method was employed to analyse 25 samples of Radix Astragali and other relative samples,including Radix Astragali slice,Radix Astragali Preparata,Hedysarum polybotrys Hand.-Mazz,Astragalus ernestii Comb.The contents of three constituents vary greatly because of the species, place of collection and season of harvesting.This method could apply to evaluate the quality of Radix Astragali and it is simple,sensitive and reliable.展开更多
目的针对炙黄芪中主要指标成分及经蜜炙转化的特征乙酰基成分,建立HPLC-PDA-ELSD测定炙黄芪中6种异黄酮及2种三萜皂苷的分析方法以及6种异黄酮的一测多评(quantitative determination analysis multi-component by a singlemarker,QAMS...目的针对炙黄芪中主要指标成分及经蜜炙转化的特征乙酰基成分,建立HPLC-PDA-ELSD测定炙黄芪中6种异黄酮及2种三萜皂苷的分析方法以及6种异黄酮的一测多评(quantitative determination analysis multi-component by a singlemarker,QAMS)法。方法选取毛蕊异黄酮7-O-β-D-葡萄糖苷(CYG)、黄芪皂苷I(AGI)分别为异黄酮和三萜皂苷类成分的内参物,并计算CYG与乙酰毛蕊异黄酮苷(CYA)、芒柄花苷(FMG)、毛蕊异黄酮(CY)、乙酰芒柄花苷(FMA)、芒柄花素(FM)及AGI与乙酰黄芪皂苷I(ATI)的相对校正因子(f_(k/s)),在不同仪器、色谱柱、柱温、体积流量上考察各成分相对校正因子的稳定性与耐用性,比较QAMS法与外标法(ESM)结果差异。结果对来自8个厂家共18批炙黄芪进行检测,PDA检测的6种异黄酮的QAMS法与ESM的结果相近,相对误差绝对值均在5%以内,表明针对异黄酮类成分建立的QAMS法准确性良好,可选用QAMS法与ESM进行质量控制;ELSD检测的2种三萜皂苷的QAMS法与ESM的结果差异明显,相对误差绝对值为0.40%~22.69%,显示针对三萜皂苷类成分建立的QAMS法不适用,应选用ESM进行质量控制。结论建立的炙黄芪中6种异黄酮及2种三萜皂苷的分析方法及6种异黄酮的QAMS法准确可靠,操作简便,可反映黄芪的蜜炙程度,为更加全面地评价炙黄芪质量提供参考,以期提升炙黄芪饮片质量。展开更多
文摘Aim To determine calycosin-7-O-β-D-glucoside,astragaloside IV and formononetin in Radix Astragali and other relative samples by HPLC-MS.Methods HPLC was carried out with Agilent 1100LC/MSD,equipped with Agilent Zorbax SB C18 column（250 mm×4.6 mm ID,5 μm） and mass spectrum detector.The mobile phase（CH3CN-H2O） was eluted in gradient mode.Results The calibration curves of calycosin-7-O-β-D-glucoside,astragaloside IV and formononetin were linear in the range of 0.031.21 μg·mL-1,0.35-13.86 μg·mL-1 and 0.38-15.22 μg·mL-1,respectively.These recoveries of samples were from 95% to 105% with RSD less than 1.5%.Conclusion The method was employed to analyse 25 samples of Radix Astragali and other relative samples,including Radix Astragali slice,Radix Astragali Preparata,Hedysarum polybotrys Hand.-Mazz,Astragalus ernestii Comb.The contents of three constituents vary greatly because of the species, place of collection and season of harvesting.This method could apply to evaluate the quality of Radix Astragali and it is simple,sensitive and reliable.
文摘目的针对炙黄芪中主要指标成分及经蜜炙转化的特征乙酰基成分,建立HPLC-PDA-ELSD测定炙黄芪中6种异黄酮及2种三萜皂苷的分析方法以及6种异黄酮的一测多评(quantitative determination analysis multi-component by a singlemarker,QAMS)法。方法选取毛蕊异黄酮7-O-β-D-葡萄糖苷(CYG)、黄芪皂苷I(AGI)分别为异黄酮和三萜皂苷类成分的内参物,并计算CYG与乙酰毛蕊异黄酮苷(CYA)、芒柄花苷(FMG)、毛蕊异黄酮(CY)、乙酰芒柄花苷(FMA)、芒柄花素(FM)及AGI与乙酰黄芪皂苷I(ATI)的相对校正因子(f_(k/s)),在不同仪器、色谱柱、柱温、体积流量上考察各成分相对校正因子的稳定性与耐用性,比较QAMS法与外标法(ESM)结果差异。结果对来自8个厂家共18批炙黄芪进行检测,PDA检测的6种异黄酮的QAMS法与ESM的结果相近,相对误差绝对值均在5%以内,表明针对异黄酮类成分建立的QAMS法准确性良好,可选用QAMS法与ESM进行质量控制;ELSD检测的2种三萜皂苷的QAMS法与ESM的结果差异明显,相对误差绝对值为0.40%~22.69%,显示针对三萜皂苷类成分建立的QAMS法不适用,应选用ESM进行质量控制。结论建立的炙黄芪中6种异黄酮及2种三萜皂苷的分析方法及6种异黄酮的QAMS法准确可靠,操作简便,可反映黄芪的蜜炙程度,为更加全面地评价炙黄芪质量提供参考,以期提升炙黄芪饮片质量。
