采用高效液相色谱法紫外检测，对饮料和酱油样品中的苯甲酸和山梨酸进行简单、高重现性的微萃取。
A simple and highly-available microextraction of benzoic and sorbic acids in beverages and soy sauce samples for high performance liquid chromatography with ultraviolet detection.
机构信息
Department of Analytical Chemistry, Institute of Chemistry, Saint-Petersburg University, St. Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.
Department of Analytical Chemistry, Institute of Chemistry, Saint-Petersburg University, St. Petersburg State University, SPbSU, SPbU, 7/9 Universitetskaya nab., St. Petersburg, 199034, Russia.
出版信息
J Chromatogr A. 2019 Mar 15;1588:1-7. doi: 10.1016/j.chroma.2018.12.030. Epub 2018 Dec 15.
A simple and highly-available air-assisted dispersive liquid-liquid microextraction procedure with organic phase solidification (AA-DLLME-OPS) was developed as new approach for pretreatment of complex sample matrix. Menthol was investigated as novel extractant for the AA-DLLME-OPS. In this procedure, a cloudy solution of fine molten menthol droplets is formed when a mixture of molten menthol and aqueous sample is rapidly aspirated into a dispenser and injected into an extraction vial. In the AA-DLLME-OPS, air bubbles promote molten menthol dispersion into aqueous sample phase. Finally, the obtained mixture is cooled and menthol phase is solidified because of the low melting point, which facilitates collection for analysis. To demonstrate the efficiency of the suggested approach, the AA-DLLME-OPS procedure was applied for the HPLC-UV determination of benzoic and sorbic acids as proof-of-concept analytes in beverages and soy sauce samples. The procedure developed provides microextraction of benzoic and sorbic acids from samples with recovery from 93 to 105% and from 96 to 101%, respectively. Under optimal experimental conditions the linear detection ranges were found to be 0.1-150 mg L for benzoic acid and 0.05-100 mg L for sorbic acid with LODs calculated from a blank test, based on 3σ, 0.03 mg L and 0.02 mg L, respectively.
一种简单且高可用性的空气辅助分散液液微萃取程序，具有有机相固化（AA-DLLME-OPS），被开发为预处理复杂样品基质的新方法。薄荷醇被研究作为 AA-DLLME-OPS 的新型萃取剂。在该程序中，当熔融薄荷醇和水样品的混合物被快速吸入分配器并注入萃取小瓶时，会形成细小的熔融薄荷醇液滴的混浊溶液。在 AA-DLLME-OPS 中，气泡促进熔融薄荷醇分散到水相样品中。最后，由于低熔点，所得混合物冷却并且薄荷醇相凝固，这便于进行分析收集。为了证明所提出方法的效率，将 AA-DLLME-OPS 程序应用于 HPLC-UV 测定饮料和酱油样品中的苯甲酸和山梨酸作为概念验证分析物。所开发的程序提供了从样品中微萃取苯甲酸和山梨酸的方法，回收率分别为 93%至 105%和 96%至 101%。在最佳实验条件下，检测范围分别为 0.1-150mg/L 用于苯甲酸和 0.05-100mg/L 用于山梨酸，LOD 基于 3σ，分别为 0.03mg/L 和 0.02mg/L，从空白测试计算。
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