加压毛细管电色谱分离检测虎杖根中蒽醌类成分

摘要

A pressurized capillary electrochromatographic (pCEC) method was developed for the determination of the main anthraquinones,including rhein,emodin,aloe-emodin,chrysophanol and physcion in root of Polygonum cuspidatum.The separation was performed on a reversed-phase EP-100-20/45-3-C1s column(total length of 45 em,effective length of 20 cm,diameter of 100 μm,ODS packing inside for 3 μm).The mobile phase was composed of 20 mmol/L NaH2PO4(pH 4.7)-acetonitrile (15 ∶ 85) at a flow rate of 0.04 mL/min.Under the optimum conditions including running voltage of + 5 kV,UV detection wavelength of 254 nm,the limits of detection (S/N=3) were in the range of 0.60-2.54 μg/mL for rhein,aloe-emodin,emodin,chrysophanol and physcion,respectively,and the linear detection ranges were 3.57-162.68 μg/mL with correlation coefficients not less than 0.998 2.The established method was used in the analysis of anthraquinones in polygonum cuspidatum with good results.The recoveries at three spiked levels ranged from 91.1％ to 101.2％,with relative standard deviations (RSD) of 0.03％-3.6％.%建立了加压毛细管电色谱法(pCEC)检测大黄酸、大黄素、芦荟大黄素、大黄酚、大黄素甲醚5种蒽醌类成分的方法,并对虎杖根中蒽醌类的成分进行分析.该方法采用EP-100-20/45-3-C18毛细管色谱柱(总长度45 cm,有效长度20 cm,直径为100 μm,ODS填料3μm)进行分离,流动相为20 mmol/LNaH2PO4(pH 4.7)-乙腈(15∶85),流动相的总流速为0.04 mL/min,分离电压为+5 kV,紫外检测波长为254 nm.结果表明,5种蒽醌类成分的检出限(S/N=3)为0.60 ～2.54 μg/mL,在3.57 ～ 162.68μg/mL范围内线性关系良好,相关系数均不小于0.998 2.将所建立的方法用于虎杖中蒽醌类成分的分析,取得良好的实验结果,在低、中、高3个加标浓度下的回收率为91.1％ ～ 101.2％,相对标准偏差(RSD)为0.03％ ～3.6％.