机构地区:[1]北京中医药大学中药学院,北京100029 [2]北京中医药大学中药分析与转化研究中心,北京100029 [3]北京中医药大学中医药研究院,北京100029 [4]石河子大学药学院,新疆石河子832002
出 处:《中草药》2019年第24期5970-5979,共10页Chinese Traditional and Herbal Drugs
基 金:国家“重大新药创制”项目(2019ZX09201004-001);国家自然科学基金项目(81774155);中央高校基本科研业务费专项资金资助项目(2019-JYB-XS-108)
摘 要:目的建立高效液相色谱-三重串联四级杆质谱(HPLC-MS/MS)联用同时测定丹荷颗粒中25种特征性成分(没食子酸、丹参素、儿茶素、绿原酸、咖啡酸、表儿茶素、芦丁、虎杖苷、金丝桃苷、紫云英苷、柚皮苷、橙皮苷、迷迭香酸、白藜芦醇、丹酚酸B、槲皮素、大黄素-8-O-β-D-葡萄糖苷、异鼠李素、大黄素、乌药碱、荷叶碱、隐丹参酮、丹参酮I、去氢荷叶碱、丹参酮IIA)含量的方法,并对其制剂批次间的一致性进行分析。方法HPLC采用Agilent Rapid Resolution HD C18色谱柱(50 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液-0.1%甲酸乙腈溶液;质谱采用动态多反应监测(dMRM)扫描模式。对25种特征性成分进行含量测定。结果建立的HPLC-MS/MS方法在10 min内完成了25种特征性成分的同时定量分析,定量限分别为异鼠李素、乌药碱、去氢荷叶碱0.025 ng/mL、大黄素、丹参酮I 0.050 ng/mL,大黄素-8-O-β-D-葡萄糖苷0.200 ng/mL,没食子酸、绿原酸、咖啡酸、表儿茶素、芦丁、金丝桃苷、紫云英苷、白藜芦醇、槲皮素、荷叶碱、丹参酮IIA 0.250 ng/mL,儿茶素、迷迭香酸、隐丹参酮0.500 ng/mL,丹参素、橙皮苷、丹酚酸B 1.000 ng/mL,虎杖苷2.000 ng/mL,柚皮苷5.000 ng/mL;且25种成分在各自质量浓度范围内线性关系良好(r>0.9901),平均加样回收率85.16%~113.46%,RSD为2.01%~8.80%。此外,该方法较为全面地囊括了丹荷颗粒中君臣佐使药材的主要成分,25种成分总量为31.49 mg/g,其中丹酚酸B(9.44 mg/g)及橙皮苷(7.60 mg/g)质量分数最高,异鼠李素(0.79μg/g)质量分数最低。经箱线图(Box-plot)分析,10个不同批次丹荷颗粒制剂中25种成分质量分数波动范围(P值)在75%<P<125%;以及统计方法分析,25种成分质量分数的RSD在2.58%~13.10%;以上结果表明10批丹荷颗粒制剂间成分含量一致性合格。结论所建立的分析方法快速、灵敏度高,结果真实可靠,能够为丹荷颗粒制剂的�Objective A high performance liquid chromatography coupled to triple quadrupole mass spectrometry method(HPLCMS/MS)was established to simultaneously determine the content of 25 characteristic components(gallic acid,tanshinol,catechin,chlorogenic acid,caffeic acid,epicatechin,rutin,polydatin,hyperin,astragalin,naringin,hesperidin,rosmarinic acid,resveratrol,salvianolic acid B,quercetin,emodin-8-O-β-D-glucoside,isorhamnetin,emodin,coclaurine,nuciferine,cryptotanshinone,tanshinone I,dehydronuciferine,tanshinone IIA)in Danhe Granules(DG),and the consistency between different batches was investigated.Methods The analysis was conducted on Agilent Rapid Resolution HD C18 column(50 mm×2.1 mm,1.8μm)with the mobile phase of 0.1%formic acid water-0.1%formic acid acetonitrile.The dynamic multi-response detection(dMRM)scanning mode was used in the mass spectrometry.Results Based on the established HPLC-MS/MS method,the simultaneous quantitative analysis of 25 characteristic components could be completed within 10 min,with the quantitative limits of isorhamnetin,coclaurine,and dehydronuciferine of 0.025 ng/mL;emodin and tanshinone I of 0.050 ng/mL;emodin-8-O-β-D-glucoside of 0.200 ng/ml;gallic acid,chlorogenic acid,caffeic acid,epicatechin,rutin,hyperin,astragalin,resveratrol,quercetin,nuciferine,tanshinone IIA of 0.250 ng/ml;catechin,rosmarinic acid,and cryptotanshinone of 0.500 ng/mL;tanshinol,hesperidin,and salvianolic acid B of 1.000 ng/mL;polydatin of 2.000 ng/mL;naringin of 5.000 ng/mL,respectively.The linear relationships of the 25 constituents within their respective mass concentrations were good,with the average recovery of 85.16%—113.46%and the RSD of 2.01%—8.80%.Furthermore,this method also included the main components named monarch,minister,assistant and guide of herbs in a relatively comprehensive way.The total content of the 25 components was 31.49 mg/g,among which the content of salvianolic acid B(9.44 mg/g)and hesperidin(7.60 mg/g)was the highest,and the content of isorhamnetin(0.79μg/g)was the lowest.
关 键 词:丹荷颗粒 HPLC-MS/MS 动态多反应监测 质量控制 一致性分析 没食子酸 丹参素 儿茶素 绿原酸 咖啡酸 表儿茶素 芦丁 虎杖苷 金丝桃苷 紫云英苷 柚皮苷 橙皮苷 迷迭香酸 白藜芦醇 丹酚酸B 槲皮素 大黄素-8-O-β-D-葡萄糖苷 异鼠李素 大黄素 乌药碱 荷叶碱 隐丹参酮 丹参酮I 去氢荷叶碱 丹参酮IIA
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