九龙化风丸中升麻素苷、5-O-甲基维斯阿米醇苷、羌活醇、异欧前胡素和细辛脂素的HPLC梯度洗脱法测定  

Determination of prim-O-glucosylcimifugin, 4'-O-β-D-glucosyl-5-O-methylvisamminol,notopterol,isoimperatorin and asarinin in Jiulong Huafeng Pills by HPLC

作　　者：高森[1] 李正翔[1] 王志涛[1] 房志仲[2] 

机构地区：[1]天津医科大学总医院,天津300052 [2]天津医科大学药学院药剂学教研室,天津市临床药物关键技术重点实验室,天津300070

出　　处：《中成药》2014年第3期541-547,共7页Chinese Traditional Patent Medicine

摘　　要：目的 采用高效液相梯度洗脱法测定九龙化风丸（防风、羌活、细辛、大黄、桔梗等）中升麻素苷、5-O-甲基维斯阿米醇苷、羌活醇、异欧前胡素和细辛脂素的量.方法 Hypersil C18色谱柱（4.6mm×150mm,5μm）,体积流量0.9 mL/min,升麻素苷和5-O-甲基维斯阿米醇苷的色谱条件,流动相A为甲醇-乙腈（2∶1）,流动相B为0.5％磷酸溶液,检测波长254 nm.羌活醇和异欧前胡素的色谱条件,流动相A为乙腈,流动相B为0.1％醋酸水溶液,检测波长310 nm,细辛脂素的色谱条件,流动相为乙腈-甲醇（85∶15）,检测波长286 nm.结果 升麻素苷和5-O-甲基维斯阿米醇苷分别在0.0146～0.2920μg （r=0.999 1）、0.0108～0.2160μg （r=0.9993）范围内进样量与峰面积呈良好的线性关系,平均加样回收率分别为97.55％、97.73％,RSD （n=6）分别为1.46％、1.18％;羌活醇和异欧前胡素分别在0.017 4 ～0.348 0 μg（r=0.999 3）、0.0128～0.2560 μg （r=0.9997）范围内进样量与峰面积呈良好的线性关系,平均加样回收率分别为97.62％、98.11％,RSD （n=6）分别为1.43％、1.39％;细辛脂素在0.012 4～0.2480 μg （r=0.999 2）范围内进样量与峰面积线性关系良好,平均加样回收率为97.65％,RSD （n=6）为1.24％.结论 该方法测定结果准确、灵敏、重复性好.AIM To develop an HPLC method for determining the contents of prim-O-glucosylcimifugin, 4′-O-β-D-glucosyl-5-O-meth-ylvisammioside, notopterol, isoimperatorin and asarinin in Jiulong Huafeng Pills （Sa- poshnikoviae Radix, Notopterygh Rhizoma et Radix, Asari Radix et Rhizoma, Rhei Radix et Rhizoma, Platycodonis Radix, etc. ）. METHODS An Hypersil Cls column was used as the chromatographic column, the flow rate was 0. 9 mL/min. For prim-O-glucosylcimifugin and 4′-O-β-D-glucosyl-5-O-methylvisamminol, the mobile phase A consisted of methanol-acetonitrile （2 ： 1）, the mobile phase B consisted of 0. 5% phosphoric acid solution, UV detection wavelength was set at 254 rim. For notopterol and isoimperatorin, the mobile phase A consisted of aceto- nitrile, the mobile phase B consisted of 0. 1% acetic acid solution, the detection wavelength was set at 310 nm.For asarinin, the mobile phase consisted of acetonitrile-methanol （85 ： 15）, the UV detection wavelength was set at 286 nm. RESULTS There was a good linear relationship between the concentration of prim-O-glucosylcimifu- gin, 4′-O-β-D-glucosyl-5-O-methylvisamminol and peak area value when the concentrations of prim-O-glucosylci- mifugin and 4′-O-β-D-glucosyl-5-O-meth-ylvisammioside were within the range of 0. 014 6 -0. 292 0μg （r = 0.999 1）, 0.0108-0.2160 μg （r=0.999 3）. The average recoveries were 97.55% （RSD=I.46%） and 97.73% （RSD =0. 1.18% ）. There was a good linear relationship between the concentration of notopterol, isoim- peratorin and peak area value when the concentrations of notopterol and isoimperatorin were within the range of 0.0174-0.348 0 μg （r =0.999 3）, 0.012 8 -0.256 0 μg （r =0.999 7）. The average recoveries were 97.62% （ RSD = 1.43% ） and 98.11% （ RSD = 1.39% ）. There was a good linear relationship between the con- centration of asarinin and peak area value when the concentrations of asarinin was within the range of 0. 012 4 - 0. 248 0 μg （r = 0. 999 2）. The average recovep/was 97.65%

关 键 词：九龙化风丸 升麻素苷 5-O-甲基维斯阿米醇苷 羌活醇 异欧前胡素 细辛脂素 梯度洗脱法 

分 类 号：R927.2[医药卫生—药学]