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
目的建立一个高准确性、高灵敏度的液相色谱一质谱联用方法，检测支气管哮喘类中成药中违禁添加的11种糖皮质激素（倍他米松，丙酸倍氯米松，氯氟舒松，醋酸泼尼松龙，氢化可的松，醋酸氟轻松，醋酸泼尼松，醋酸曲安奈德，醋酸可的松，...目的建立一个高准确性、高灵敏度的液相色谱一质谱联用方法，检测支气管哮喘类中成药中违禁添加的11种糖皮质激素（倍他米松，丙酸倍氯米松，氯氟舒松，醋酸泼尼松龙，氢化可的松，醋酸氟轻松，醋酸泼尼松，醋酸曲安奈德，醋酸可的松，氢化泼尼松，醋酸地塞米松）。方法色谱条件为Waters×Terra MS C18色谱柱（2．1mm×150mm，5μm），柱温35℃，流动相以0．1％甲酸10mmol／L乙酸铵溶液-乙腈进行梯度洗脱，体积流量为0．25mL／min。质谱条件为以电喷雾离子源正离子模式进行质谱数据采集。结果在建立的色谱条件下，11种糖皮质激素有良好的分离，且对其定性定量检出，线性范围良好，加样回收率为90％～110％。结论该法操作简便、快捷、高灵敏度、高准确性等特点，可同时对中成药中非法添加多种糖皮质激素进行定性定量分离检测。展开更多
目的：建立一种远志中远志酮Ⅲ和3,6＇-二芥子酰基蔗糖含量的HPLC-MS/MS分析方法。方法：采用ZORBAX Eclipse plus C18色谱柱,（4.6 mm×100 mm,3.5μm）,流动相乙腈-0.1%甲酸水（28∶72）,流速0.3 m L·min^-1,进样量10μL,...目的：建立一种远志中远志酮Ⅲ和3,6＇-二芥子酰基蔗糖含量的HPLC-MS/MS分析方法。方法：采用ZORBAX Eclipse plus C18色谱柱,（4.6 mm×100 mm,3.5μm）,流动相乙腈-0.1%甲酸水（28∶72）,流速0.3 m L·min^-1,进样量10μL,柱温20℃。质谱条件：电喷雾负离子化模式,多反应监测模式（MRM）,检测离子对分别为m/z 567.2~345.1（远志酮Ⅲ）,m/z 753.3~205.1（3,6＇-二芥子酰基蔗糖）。结果：两种成分的线性关系良好,分析过程只需6 min。远志酮Ⅲ的日内精密度和日间精密度的RSD分别为2.2%,2.5%,回收率为96.1%~101.7%（RSD 2.4%）;3,6＇-二芥子酰基蔗糖的日内精密度和日间精密度的RSD分别为2.3%,2.4%,回收率为95.7%~101.4%（RSD 2.0%）。结论：该方法快速、灵敏、选择性好,适合远志中远志酮Ⅲ和3,6＇-二芥子酰基蔗糖的定量分析。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.
文摘目的建立一个高准确性、高灵敏度的液相色谱一质谱联用方法，检测支气管哮喘类中成药中违禁添加的11种糖皮质激素（倍他米松，丙酸倍氯米松，氯氟舒松，醋酸泼尼松龙，氢化可的松，醋酸氟轻松，醋酸泼尼松，醋酸曲安奈德，醋酸可的松，氢化泼尼松，醋酸地塞米松）。方法色谱条件为Waters×Terra MS C18色谱柱（2．1mm×150mm，5μm），柱温35℃，流动相以0．1％甲酸10mmol／L乙酸铵溶液-乙腈进行梯度洗脱，体积流量为0．25mL／min。质谱条件为以电喷雾离子源正离子模式进行质谱数据采集。结果在建立的色谱条件下，11种糖皮质激素有良好的分离，且对其定性定量检出，线性范围良好，加样回收率为90％～110％。结论该法操作简便、快捷、高灵敏度、高准确性等特点，可同时对中成药中非法添加多种糖皮质激素进行定性定量分离检测。
