摘要
目的:建立胶束电动毛细管色谱二极管阵列检测法(MEKC-DAD)测定山茱萸饮片中獐牙菜苷、马钱苷含量的方法。方法:应用未涂渍标准熔融石英毛细管(75μmi.d.×64.5cm,有效长度56cm),检测波长:240nm;压力进样:5kPa×8s;分离电压:10kV;柱温:18℃;运行缓冲液:50mmol/L硼砂-40mmol/L十二烷基硫酸钠-5%乙腈(pH9.5)。并考察了缓冲溶液浓度、表面活性剂浓度、有机溶剂、缓冲溶液pH、运行电压、运行温度等因素对待测物质分离的影响。结果:獐牙菜苷、马钱苷分别在19.25~192.5,121~1210mg/L范围内线性关系良好(r=0.9989,0.9987);回收率分别为100.38%(RSD2.80%),100.41%(RSD2.98%);最低检测限分别为4.81、28.92mg/L,最低定量限分别为16.04、96.41mg/L。结论:方法简便、灵敏,重复性与加样回收率良好,可作为山茱萸质量分析的新方法。
AIM: To establish a micellar electrokinetic chromatography method with diode array detection (MEKC-DAD) for determining sweroside and loganin in Fructus Corni processed with wine.METHODS: MEKCDAD was carried out in a buffer solution of 50 mmol/L borax solution-40 mmol/L SDS-5% -acetonitrile (pH 9.5);running voltage was 10 kV;column temperature was at 18 ℃;the detection wavelength was set up 240 nm.The effects of the applied voltage,detection wavelength,and the pH of buffer,the concentration of buffer,surfactant and acetonitrile were investigated.RESULTS: The linear libration range fell within 19.25-192.5 mg/L(r = 0.998 9)for sweroside,121-1 210 mg/L(r = 0.998 7)for loganin.The recoveries of sweroside and loganin were 100.38% (RSD 2.80% ) mg/L and 100.41% (RSD 2.98% ),respectively.The limits of detection of sweroside and loganin were 16.04 mg/L and 96.41 mg/L,respectively.The limits of quantitation of sweroside and loganin were 4.81 mg/L and 28.92 mg/L respectively.CONCLUSION: The method is a simple,sensitive and reproducible approach.More importantly,results indicate that the new method shows promising prospect for quality control of Fructus Corni and its processed products.
出处
《中成药》
CAS
CSCD
北大核心
2010年第6期970-973,共4页
Chinese Traditional Patent Medicine
基金
国家自然科学基金(30873438)
江苏省中药炮制重点实验室开放课题(ZYPZ007)