微乳液相色谱直接进样测定大鼠血清中大黄素的含量

Determination of rat serum emodin level by microemulsion liquid chromatography with direct sample loading

目的考察血清直接进样的可行性,建立大鼠血清中大黄素的微乳液相色谱直接进样测定法。方法采用Hypersil BDS C185μm(4.6mm×150mm)色谱柱,以微乳(3.3%十二烷基硫酸钠(SDS)w/V-6.6%正丁醇V/V-1.0正辛烷V/V-水)为流动相,检测波长254nm,血清经微孔滤膜过滤后直接进样。结果大黄素在0.333～5.32μg·ml-1范围与峰面积呈良好线性关系,平均回收率为99.65%,RSD为3.60%,最低定量限为0.1386μg·ml-1。结论采用微乳流动相,可直接进样测定血清样品中大黄素的含量,方法简单、准确、快速。

Objective To establish a microemulsion liquid chromatography system with direct sample loading for determining the serum level of emodin in rats. Methods The separation was performed on C18 column （Hypersil BDS,5 μm,150 mm×4.6 mm） with the microemulsion mobile phase consisting of 3.3% （w/V） SDS,6.6% （V/V） n-butyl alcohol,and 1.0% （V/V） octane and water. The flow rate was 1.0 ml/min and the detection wavelength was 254 nm. Results The linear range of emodin detection was 0.333-5.32 μg/ml. The average recovery was 99.65% with a RSD of 3.60%. The limit of quantification was 0.1386 μg/mL. Conclusion Microemulsion liquid chromatography system with direct sample loading allows simple,accurate and rapid determination of emodin in rat serum.