College of Chemistry, Liaoning University, 66 Chongshan Middle Road, Shenyang 110036, China; Department of Mechanical and Power Engineering, Yingkou Institute of Technology, Yingkou 115014, China.
College of Chemistry, Liaoning University, 66 Chongshan Middle Road, Shenyang 110036, China.
Talanta. 2019 Jul 1;199:212-219. doi: 10.1016/j.talanta.2019.02.065. Epub 2019 Feb 18.
A simple, rapid and sensitive method based on in situ derivatization combined with magnetic ionic liquid (MIL)-dispersive liquid-liquid microextraction (DLLME) was developed for the determination of biogenic amines (BAs). Six BAs (tryptamine, phenylethylamine, histamine, tyramine, spermidine, and spermine) were in situ derivatized with dansyl chloride (DNS-Cl), extracted by MIL-DLLME, and then chromatographed by high-performance liquid chromatography with ultraviolet detection (HPLC-UV). This MIL trihexyltetradecylphosphonium tetrachlorocobalt (II) [P][CoCl] was explored as the extraction solvent with the advantages of magnetic susceptibility, hydrophobicity and mobile phase compatibility. Furthermore, the MIL was designed to reduce hydrolysis in aqueous solvent as well as decrease absorbance when submitted to HPLC. In order to obtain optimized extraction efficiency, the MIL mass, the volume of derivatizing agent, the type and volume of disperser, the derivatizing and extraction time, and pH of sample solution were investigated. The proposed method was successfully applied for the analysis of wine and fish samples, and the recoveries of analytes achieved were in the range of 93.2-103.1% and 94.5-102.3%, respectively. The limits of detection/quantification for wine and fish samples were in the range of 1.3-3.9/4.1-9.9 μg/L and 1.2-3.8/3.9-9.6 μg/kg, respectively. Additionally, good reproducibility with relative standard deviations lower than 4.9% (n = 5) was obtained for the analysis of wine and fish samples. The in situ DNS-Cl derivatization and MIL-DLLME method was an efficient, rapid, environmental friendly microextraction approach for the determination of BAs in foodstuffs.
建立了一种基于原位衍生结合磁性离子液体（MIL）-分散液液微萃取（DLLME）的简单、快速、灵敏的方法，用于测定生物胺（BAs）。6 种生物胺（色胺、苯乙胺、组氨酸、酪胺、亚精胺和精胺）与丹磺酰氯（DNS-Cl）原位衍生，用 MIL-DLLME 萃取，然后用高效液相色谱-紫外检测（HPLC-UV）进行色谱分析。该 MIL 三己基十四烷基膦四氯合钴（II）[P][CoCl]被探索为萃取溶剂，具有磁导率、疏水性和与流动相的兼容性等优点。此外，设计了 MIL 以减少在水溶剂中的水解以及在提交给 HPLC 时的吸光度。为了获得最佳的萃取效率，考察了 MIL 质量、衍生化剂体积、分散剂类型和体积、衍生化和萃取时间以及样品溶液的 pH 值。该方法成功应用于葡萄酒和鱼类样品的分析，分析物的回收率范围分别为 93.2-103.1%和 94.5-102.3%。葡萄酒和鱼类样品的检出限/定量限范围分别为 1.3-3.9/4.1-9.9μg/L 和 1.2-3.8/3.9-9.6μg/kg。此外，对于葡萄酒和鱼类样品的分析，相对标准偏差（RSD）低于 4.9%（n=5），具有良好的重现性。原位 DNS-Cl 衍生和 MIL-DLLME 方法是一种高效、快速、环境友好的微萃取方法，用于测定食品中的 BAs。
