CAJ | 학술논문

建立了在线扫集-胶束电动毛细管色谱法同时分离测定活血通脉片中阿魏酸和原儿茶醛含量的方法.讨论了pH值、十二烷基磺酸钠(SDS)浓度、电压、有机溶剂、进样时间和背景电解质组成对分离效果的影响.结果表明:采用未涂层熔融石英毛细管 ,以20 mmol/L磷酸二氢钠、140 mmol/L SDS为电泳缓冲液(含16%甲醇,pH 2.2),在优化条件下,阿魏酸和原儿茶醛在19 min内出峰,峰面积RSD均小于5%,其线性范围分别为0.67 ～21.4、0.72 ～23 mg/L,回收率分别为94% ～108%、91% ～106%,检出限(S/N=3)分别达55.5、34.8 μg/L.与胶束电动毛细管色谱相比,在线扫集-胶束电动毛细管色谱分离效果稳定,重现性好.该方法用于活血通脉片中阿魏酸、原儿茶醛含量的测定,结果满意.
건립료재선소집-효속전동모세관색보법동시분리측정활혈통맥편중아위산화원인다철함량적방법.토론료pH치、십이완기광산납(SDS)농도、전압、유궤용제、진양시간화배경전해질조성대분리효과적영향.결과표명:채용미도층용융석영모세관 ,이20 mmol/L린산이경납、140 mmol/L SDS위전영완충액(함16%갑순,pH 2.2),재우화조건하,아위산화원인다철재19 min내출봉,봉면적RSD균소우5%,기선성범위분별위0.67 ～21.4、0.72 ～23 mg/L,회수솔분별위94% ～108%、91% ～106%,검출한(S/N=3)분별체55.5、34.8 μg/L.여효속전동모세관색보상비,재선소집-효속전동모세관색보분리효과은정,중현성호.해방법용우활혈통맥편중아위산、원인다철함량적측정,결과만의.
A sweeping-micellar electrokinetic chromatographic(sweeping -MEKC) method was used for the simultaneous separation and determination of ferulic acid and protocatechuic aldehyde.Effect of pH,concentration of sodium dodecyl sulfate(SDS) and methanol,injection time,injection voltage,composition and concentration of background electrolyte on separation efficiency were optimized.The result indicated that a best separation of ferulic acid and protocatechuic aldehyde was obtained on an uncoated fused silica capillary column(60 cm×50 μm,effective length 47 cm) by using the background electrolyte containing 140 mmol/L SDS,20 mmol/L NaH_2PO_4 and 16%(by volume) methanol at pH 2.2 with a constant temperature of 25 ℃ and applied voltage of -20 kV. The detection wavelength was set at 316 nm,sample injection time and injection height were selected to be 100 s and 16 cm,respectively.Under the optimum conditions,the separation of ferulic acid and protocatechuic aldehyde was performed within 19 minutes with relative standard deviation(RSDs) of peak area less than 5%.The calibration curves showed good linearity in the range of 0.67 -21.4 mg/L for ferulic acid and 0.72-23 mg/L for protocatechuic aldehyde,with detection limits(S/N=3) of 55.5 μg/L and 34.8 μg/L, respectively. The spiked recoveries were 94%-108% and 91%-106%.Compared with MEKC method,the sweeping-MEKC method showed high separation efficiency, good sensitivity, and was applied in the simultaneous separation and determination of ferulic acid and protocatechuic aldehyde with satisfactory results.