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两步压力注射辅助在线富集-胶束电动色谱亲和胶束扫除法测定食品中的除草剂。

Two-step pressure injection-assisted online enrichment of herbicides from foods with affinity micelle sweeping by micellar electrokinetic chromatography.

机构信息

College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 311121, China.

College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 311121, China.

出版信息

J Chromatogr A. 2023 Sep 13;1706:464258. doi: 10.1016/j.chroma.2023.464258. Epub 2023 Aug 1.

Abstract

A novel online two-step pressure injection-assisted stacking preconcentration method, which involves sweeping and affinity micelles in micellar electrokinetic chromatography was developed to simultaneously measure various organic anions. The micellar solution was a mixed solution that contained 0.3 mM didodecyldimethylammonium bromide and 20 mM borax. After the micellar solution was injected for 60 s, the tested analytes prepared in 20 mM borax were introduced into the capillary for 150 s. The key experimental factors that influenced the separation and sensitivity were investigated and optimized, including the concentration and injection time of the micellar solution, the concentration of borax in the sample solution, the concentration of sodium dodecyl sulfate and borax in the background electrolyte (BGE), the content of acetonitrile in the BGE and the injection time of the sample solution. Compared with typical injection methods, this method achieved sensitivity enhancement factors ranging from 85 to 97 under optimized conditions. Good linearity for matrix-matched calibration was established for all analytes with R values of 0.9986-0.9996. The intraday (n = 6) and interday (n = 6) precisions of the method were less than 2.85% when expressed as relative standard deviations. When the method was applied to analyze rice and dried ginger samples, analyte recoveries ranged from 85.81% to 106.59%. Through sweeping and affinity micelles, stacking preconcentration method was successfully employed to analyze trace amounts of fenoprop and 2,4-dichlorophenoxyacetic acid in rice and dried ginger samples.

摘要

一种新颖的在线两步压力注射辅助堆积浓缩方法,涉及胶束电动色谱中的扫集和亲和胶束,用于同时测量各种有机阴离子。胶束溶液是一种混合溶液,包含 0.3mM 双十二烷基二甲基溴化铵和 20mM 硼砂。在注入胶束溶液 60s 后,将在 20mM 硼砂中制备的测试分析物引入毛细管中 150s。研究并优化了影响分离和灵敏度的关键实验因素,包括胶束溶液的浓度和注入时间、样品溶液中硼砂的浓度、背景电解质(BGE)中十二烷基硫酸钠和硼砂的浓度、BGE 中乙腈的含量和样品溶液的注入时间。与典型的注入方法相比,在优化条件下,该方法实现了 85%至 97%的灵敏度增强因子。所有分析物均建立了基质匹配校准的良好线性关系,相关系数(R)为 0.9986-0.9996。该方法日内(n=6)和日间(n=6)精密度以相对标准偏差表示均小于 2.85%。当该方法应用于分析稻米和干姜样品时,分析物的回收率在 85.81%至 106.59%之间。通过扫集和亲和胶束,成功地将堆积浓缩方法用于分析稻米和干姜样品中痕量的 Fenoprop 和 2,4-二氯苯氧乙酸。

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