Yang Xiumin, Hao Lin, Zhang Shuaihua, Wang Chun, Wang Zhi
Department of Chemistry, College of Science, Agricultural University of Hebei Baoding 071001 China
RSC Adv. 2018 Feb 20;8(15):7949-7955. doi: 10.1039/c7ra11553a. eCollection 2018 Feb 19.
A novel on-line two-step stacking preconcentration method by sweeping plus micelle to solvent stacking in capillary zone electrophoresis was developed for the simultaneous determination of three organic anions (vanillic acid, ferulic acid and cinnamic acid) in . Hexadimethrine bromide was used for electroosmotic flow reversal. The main experimental parameters that affected the separation and sensitivity were investigated and optimized. The best separation was achieved in 50 mM ammonium acetate (pH 12.0) containing 50% methanol (v/v) under a negative voltage of 20 kV. The micellar solution was a mixed solution comprised of 12 mM cetyltrimethyl ammonium bromide and 20 mM ammonium acetate. After injecting a short plug (0.5 psi, 30 s) of micellar solution, the sample was introduced into the capillary at 0.5 psi for 45 s. Under the optimal conditions, the sensitivity enhancement factors obtained by the developed method were between 42 and 77. The intra-day ( = 6) and inter-day ( = 5) precisions of the method expressed as their relative standard deviations were found to be less than 7.2%. The sample was pulverized and then refluxed in 95% ethanol and filtered. After an aliquot of the extractant was dried, it was reconstituted in 20 mM ammonium acetate for capillary electrophoresis analysis. The recoveries of the analytes by this method for the analysis of were in the range of 94.4% to 108.4%.
开发了一种新颖的在线两步堆积预浓缩方法,即毛细管区带电泳中的扫集加胶束到溶剂堆积,用于同时测定[具体样本]中的三种有机阴离子(香草酸、阿魏酸和肉桂酸)。使用溴化己二甲铵进行电渗流反转。研究并优化了影响分离和灵敏度的主要实验参数。在20 kV负电压下,于含50%甲醇(v/v)的50 mM醋酸铵(pH 12.0)中实现了最佳分离。胶束溶液是由12 mM十六烷基三甲基溴化铵和20 mM醋酸铵组成的混合溶液。注入一小段胶束溶液(0.5 psi,30 s)后,以0.5 psi将样品引入毛细管45 s。在最佳条件下,所开发方法获得的灵敏度增强因子在42至77之间。该方法的日内(n = 6)和日间(n = 5)精密度以相对标准偏差表示,均小于7.2%。将[具体样本]粉碎,然后在95%乙醇中回流并过滤。取一份萃取剂干燥后,用20 mM醋酸铵复溶用于毛细管电泳分析。该方法对[具体样本]分析时,分析物的回收率在94.4%至108.4%范围内。