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机构地区:[1]西南民族大学少数民族药物研究所,四川成都610041
出 处:《中成药》2014年第12期2526-2531,共6页Chinese Traditional Patent Medicine
基 金:国家十二五科技支撑计划(2012BAI27B07);西南民族大学硕士点建设项目(2014XWD-S0703)
摘 要:目的建立二十一味寒水石丸(寒水石、木香、牛黄、藏木香等)中木香烃内酯、去氢木香内酯、胆酸、土木香内酯和异土木香内酯的RP-HPLC测定方法。方法二十一味寒水石丸甲醇提取液的测定在迪马Diamonsil-2 C18(4.6 mm×250 mm,5μm)色谱柱进行,流动相分别为乙腈-水(65∶35)、甲醇-0.1%醋酸溶液(75∶25)和乙腈-0.1%磷酸水(52∶48);体积流量分别为1.0、0.8、1.0 m L/min;柱温均为30℃;其中木香烃内酯和去氢木香内酯检测使用二极管阵列检测器,检测波长225 nm;胆酸检测使用蒸发光散射检测器,漂移管温度90℃,氮气体积流量为1.6 L/min;土木香内酯和异土木香内酯的检测波长为220 nm。结果木香烃内酯、去氢木香内酯、胆酸、土木香内酯和异土木香内酯线性范围分别为0.043 5-0.435μg(r=0.999 8)、0.045-0.45μg(r=0.999 9)、0.506 5-2.533μg(r=0.999 9)、0.64-2.4μg(r=0.999 3)、0.64-2.4μg(r=0.999 9);平均回收率分别为99.5%、99.7%、99.8%、99.3%、99.6%;RSD分别为0.8%、0.9%、1.3%、0.7%、1.1%(n=9)。结论本方法可用于二十一味寒水石丸中5个成分的定量测定。AIM To establish the method for determining costunolide,dehydrocostus lactone,cholic acid,alantolacton,and isoalantolactone in Ershiyiwei Hanshuishi Pills( Hanshuishi,Aucklandia lappa Decne.,Bostaurus domesticus Gmelin,Inula race mosa Hook. J,etc). METHODS The samples were separated on Diamonsil-2 C18column( 4. 6 mm × 250 mm,5 μm) using acetonitrile-water( 65 ∶ 35),methanol-0. 1% acetic acid( 75 ∶25) and acetonitrile-0. 1% phosphoric acid( 52 ∶ 48) as mobile phase with the flow rate of 1. 0 m L / min,0. 8m L / min and 1. 0 m L / min,respectively. The column temperature was kept at 30 ℃. 2996 PDA detector was used for costunolide and dehydrocostus lactone. The detection wavelength was 225 nm and ELSD was used for cholic acid. The flow rate of nitrogen was 1. 6 L / min and the temperature of drift tube was 90 ℃. The detection wavelength was 220 nm for lantolactone and isoalantolactone. RESULTS The linear ranges for costunolide,dehydrocostus,cholic acid,alantolactone and isoalantolactone were 0. 043 5- 0. 435 μg( r = 0. 999 8),0. 045- 0. 45 μg( r = 0. 999 9),0. 506 5- 2. 533 μg( r = 0. 999 9),0. 64- 2. 4 μg( r = 0. 999 3) and 0. 64- 2. 4 μg( r =0. 999 9),respectively. The average recovery rates were 99. 5%,99. 7%,99. 8%,99. 3% and 99. 6%,respectively. The RSD were 0. 8%,0. 9%,1. 3%,0. 7% and 1. 1%,respectively. CONCLUSION This method is suitable for the quantitative determination of Ershiyiwei Hanshuishi Pills.
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