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机构地区:[1]承德医学院附属医院,河北承德067000 [2]承德市北方医院,河北承德067000 [3]承德市疾病控制中心,河北承德067000 [4]承德医学院中医研究所,河北承德067000
出 处:《时珍国医国药》2008年第1期61-63,共3页Lishizhen Medicine and Materia Medica Research
基 金:河北省卫生厅医药开发重大项目(No.04006)
摘 要:目的采用酸性染料比色法测定北豆根提取物中北豆根总碱(TAMD)的含量,采用高效液相色谱(HPLC)法测定蝙蝠葛碱(Dauricine)的含量。方法溴甲酚绿在无水甲醇(pH=6)中,可与TAMD直接络合生成绿色化合物,用于比色测定,最大吸收波长为620nm。HPLC法,色谱柱:Discovery C18柱;流动相:乙腈:水:磷酸=16:84:0.15;流速:0.5ml·min^-1;检测波长:208nm。结果酸性染料比色法:线性范围为6~40μg·ml^-1,r=0.9998(n=7),平均加样回收率为99.18%,RSD=0.74%;HPLC法:线性范围为0.01~0.1mg·ml^-1,r=0.9998(n=7),平均加样回收率为98.32%,RSD=0.94%。结论建立的方法灵敏、准确、重现性好,可作为北豆根提取物中TAMD和蝙蝠葛碱的含量分析方法。Objective To establish an acid dye eolorimetric method for determination of total alkaloid in Menispermum dauricum (TAMD), an HPLC method for determination of Dauricine . Methods TAMD produced green combination with bromocresol green in the condition of dehydrated ethanol , according to this characteristic, acid dye colorimetry was established. HPLC method:The separation was carried out on a Discovery -C18 column(250 mm ×4.6 mm,5 μm) , the mobile phase was acetonitrile -water - phosphoric acid( 16: 84:0.15 ) , the flow rate was 0.5 ml · min^ -1 , and detection wavelength was 208 nm. Results Acid dye colorimetric method:The linear range was 6 -40 μg · ml^-1 , r =0.999 8(n =7) , the average recovery was 99.18% with the RSD of 0.74%. HPLC method:The linear range was 0.01 - 0.1 mg · ml^-1 , r = 0. 999 8 ( n = 7) ,the average recovery was 98.32% with the RSD of 0.94%. Conclusion This method is sensitive, accurate and reproducible, and can be used in analyzing the content of TAMD and Dauricine in RM extract.
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