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作 者:姜韧[1] 梁爱君[2] 魏萍[2] 徐冰心 刘刚 谭生建
机构地区:[1]中国人民解放军第306医院,药剂科,北京100101 [2]中国人民解放军总后勤部卫生部药品仪器检验所,北京100071 [3]不详
出 处:《解放军药学学报》2003年第6期443-445,共3页Pharmaceutical Journal of Chinese People's Liberation Army
摘 要:目的 建立高效液相色谱法测定解毒固本颗粒中大黄素和大黄酚含量的方法。方法 MZC18分析色谱柱 (4 .6mmID× 2 5 0mm ,粒径 5 μm) ,流动相A :10 %乙腈 (含 0 .5 %三乙胺 ,磷酸调pH3.0 ) ;B :85 %乙腈 (含 0 .5 %三乙胺 ,磷酸调pH3.0 )。梯度洗脱程序 :1~ 11min ,A :4 0 %~ 0 ;B :6 0 %~ 10 0 % ,流速 1.5ml/min。检测波长 4 33nm ;结果 大黄素回归方程Y =- 0 .0 0 14 75+0 .0 0 0 0 0 0 0 2 6 33X ,r =0 .9999,线性范围 0 .0 16 6 4~ 0 .6 6 5 4 μg ;大黄酚回归方程Y =- 0 .0 0 346 4 +0 .0 0 0 0 0 0 0 2 4 82X ,r =0 .9999,线性范围 0 .0 2 4 4 7~ 0 .9789μg。大黄素和大黄酚平均回收率分别为 96 .2 % (RSD =4 .7% )和 97.4 % (RSD =2 .1% )。结论 该方法操作简便 ,测定结果准确可靠 ,可用于测定解毒固本颗粒中大黄素和大黄酚含量。Aim To establish a HPLC method to determine the concentration of emodin and chrysophanol in jieduguben granules.Methods The chromatographic conditions include column MZ C 18 ,gradient elution mobile phase:A:10% acetonitrile with 0.5% triethylamine,pH was adjusted to 3.0 by phosphoric acid.B:85% acetonitrile with 0.5% triethylamine,pH was adjusted to 3.0 by phosphoric acid,the gradient elution pocess:1~11min,A:40%~0,B:60%~100%,flow rate 1.5ml/min,wavelength 433nm.Results The regression equation of emodin was Y=-0.001 475+0.000 000 026 33X(r=0.999 9),and the linear range was 0.0166 4~0.665 4μg.The regression equation of chrysophanol was Y=-0.003 464+0.000 000 024 82X,r=0.999 9,and the linear range was 0.024 47~0.978 9μg.The average recovery of emodin was 96.2% (RSD=4.7%),the average recovery of chrysophanol was 97.4% (RSD=2.1%).Conclusion The method was sensitive,rapid and accurate.
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