大体积样品堆积-微乳液胶束电动色谱法测定5种黄酮类化合物

Determination of Five Flavonoid Compounds by Microemulsion Electrokinetic Chromatrography with Large Volume Sample Stacking

本文利用大体积样品堆积-微乳液胶束电动色谱法(LVSS-MEEKC)测定5种黄酮类化合物。采用LVSS对样品进行富集,最佳条件为:分离电压20kV,进样时间20.7kPa×55s,堆积时间1.25 min,堆积电压-20kV。最佳MEEKC条件为:以20mmol/L硼砂-40 mmol/L NaH2PO4(pH=9.0)+0.3%十二烷基硫酸钠(SDS)+1%乙酸乙酯+2%正丁醇为运行缓冲液,分离电压20kV,检测波长214nm。在最优化的分离条件和富集条件下,5种黄酮类化合物在12min内得到基线分离,5种成分的检测限(3倍信噪比)低至ng/mL级。将所建立的方法用于人尿加标样品的测定,加标回收率在92.50%~110.0%之间。

In this paper, five flavonoids were determined by largevolume sample stacking （LVSS） with microemulsion electrokinetic chromatrography（MEEKC）, and the new method was established for the determina ction of flavonoids in human urine samples. The best LVSS condition was.separation voltage 20 kV,injection time 20.7 kPaX55 s,the deposition time 1.25 min,a bulk voltage of --20 kV. The most suitable buffer composition was 20 mmol/L borate-40 mmol/L phosphate buffer（pH= 9.0） with 0.3% SDS,1 G ethyl acetate and 20% butyl alcohol, separation voltage was 20 kV, detection wavelength was 214 nm. Under the optimum LVSS-MEEKC conditions, the five flavonoids was baseline separated in 12 min and the detection limits of the five components（3 times the signal to noise ratio） could be as low as ng/mL level. The established method was used for the determination of human urine samples and the spiked recoveries were ranged from 92.50G to 110.0%. The proposed LVSS-MEEKC method would improve the detection sensitivity and reduce interference with the biological sample matrix.