UPLC法同时测定感冒解痛散中10种成分的含量

Simultaneous determination of 10 components in Ganmaojietong Powder by UPLC

目的建立能同时测定感冒解痛散中芹菜素、槲皮素、木犀草素、欧前胡素、异欧前胡素、橙皮苷、川陈皮素、苍术素、甘草苷和盐酸麻黄碱10种成分的超高效液相色谱法(UPLC)。方法采用Waters XTERRA C 18(100 mm×2.1 mm,1.6μm)色谱柱,流动相:乙腈-8 mL·L^(-1)磷酸(含0.1 mL·L^(-1)三乙胺),梯度洗脱;流速为0.2 mL·min^(-1);检测波长分别为:237(甘草苷)、215(盐酸麻黄碱)、360(芹菜素、槲皮素、木犀草素、橙皮苷)、326(川陈皮素)、249(欧前胡素、异欧前胡素)和336 nm(苍术素);柱温:35℃;进样量:2μL。结果10种成分检测质量浓度线性范围分别为1.448~11.58、3.104~24.83、1.403~72.62、9.078~77.08、9.635~25.99、3.249~37.33、4.667~25.08、3.136~12.11、1.514~10.89、1.362~24.83μg·mL^(-1)(r值均在0.9992~0.9998)之间;精密度、24 h稳定性、重复性实验的RSD值均小于2.0%(n=6);平均回收率分别为98.51%、99.49%、99.63%、100.62%、100.95%、99.95%、99.28%、99.73%、100.04%、99.02%(RSD<2.0%,n=6)。结论所建立的方法简便、准确、重复性好,可用于感冒解痛散的质量控制。

Objective To develop a ultra high performance liquid chromatography(UPLC)method for simultaneous determination of 10 components in Ganmaojietong Powder,including apigenin,quercetin,luteolin,imperatorin,isoimperatorin,hesperidin,nobiletin,atractylodin,liquiritin and ephedrine hydrochloride.Methods The chromatographic analysis was carried out on a Waters XTERRA C 18 column(100 mm×2.1 mm,1.6μm)with the mobile phase consisted of acetonitrile-8 mL·L^(-1)phosphoric acid(containing 0.1 mL·L^(-1)triethylamine).The flow rate was 0.2 mL·min^(-1)with gradient elution.The detection wavelength was set at 237 nm for liquiritin,215 nm for ephedrine hydrochloride,360 nm for apigenin,quercetin,luteolin and hesperidin,326 nm for nobiletin,249 nm for imperatorin and isoimperatorin,and 336 nm for atractylodin.The column temperature was set at 35℃and the injection volume was 2μL.Results The linear ranges of the 10 components detection mass concentration were 1.448-11.58,3.104-24.83,1.403-72.62,9.078-77.08,9.635-25.99,3.249-37.33,4.667-25.08,3.136-12.11,1.514-10.89,1.362-24.83 mg·g-1(r within 0.9992-0.9998).The RSDs of precision,reproducibility and stability tests(24 h)were all lower than 2.0%(n=6).The average recoveries were 98.51%、99.49%、99.63%、100.62%、100.95%、99.95%、99.28%、99.73%、100.04%、99.02%(RSD<2.0%,n=6),respectively.Conclusion The method is simple,accurate and reproducible,and can be used for the quality control of Ganmaojietong Powder.