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作 者:王桂英[1] 戴学文[2] 王姿婧[2] 刘青[2] 房志仲[2]
机构地区:[1]天津市中医药研究院附属医院药学部,天津300120 [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:《中国药房》2013年第31期2951-2953,共3页China Pharmacy
摘 要:目的:建立测定散风解表颗粒中黄芩苷和腺苷含量的方法。方法:采用高效液相色谱法。色谱柱为TIANHEKromasilC18(200mm×4.6mm,5μm),柱温为室温,流速为0.8ml/min,进样量为20μl。黄芩苷测定的流动相为甲醇-水(55∶45,V/V,加冰乙酸调pH值至3.10),检测波长为277nm;腺苷测定的流动相为0.04mol/LNaH2PO4-乙腈(94∶6,V/V),检测波长为260nm。结果:黄芩苷的质量浓度在70~190μg/ml范围内与其峰面积积分值呈良好线性关系(r=0.9999);低、中、高加入量对应的平均回收率分别为101.82%、102.53%、97.40%,RSD分别为0.96%、0.50%、1.44%(n均为3)。腺苷的质量浓度在5~65μg/ml范围内与其峰面积积分值呈良好线性关系(r=0.9998);低、中、高加入量对应的平均回收率分别为99.58%、99.36%、101.59%,RSD分别为1.23%、1.20%、1.12%(n均为3)。结论:该方法简便、准确、可靠,可作为散风解表颗粒的质量控制方法。OBJECTIVE: To establish the method for the content determination of baicalin and adenosine in Sanfeng jiebiao granules. METHODS: HPLC method was adopted. The determination was performed on TIANHE~ Kromasil Ct8(200 minx4.6 mm, 5 μm) column at flow rate of 0.8 ml/min; the column temperature was room temperature and sample size was 20 μl. The mobile phase of baicalin was methanol-water (55 : 45, V/V, pH adjusted to 3.10 using glacial acetic acid), and the detection wavelength was set at 277 nm; and the mobile phase of adenosine was 0.04 mol/L monosodium phosphate-acetonitrile(94 : 6, V/V), and the de- tection wavelength was set at 260 nm. RESULTS:The linear range of baicalin were 70-190 μg/ml(r=0.999 9); average recoveries were 101.82% (RSD=0.96%, n=3), 102.53% (RSD=0.50%, n=3) and 97.40% (RSD=1.44%, n=3) for low, medium and high concentrations. The linear range of adenosine were 5-65 μg/ml(r=0.999 8); average recoveries were 99.56% (RSD=1.23%, n=3), 99.36% (RSD=1.20%, n=3) and 101.59% (RSD= 1.12%, n=3) for low, medium and high concentrations. CONCLU- SIONS : The method is simple, accurate and reliable, and it can be used for the quality control of Sanfeng jiebiao granules.
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