MEKC-DAD测定山茱萸饮片中獐牙菜苷和马钱苷含量

Determination of sweroside and loganin in Fructus Corni and its processed products by MEKC-DAD

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.