Su Mingming, He Yongke, Zhang Ning, Lv Meiheng, Xu Xu
Department of Chemistry, Liaoning University, Chongshan Middle Road No.60, Huanggu Dis., Shenyang, 110036, P. R. China.
Technology Center, Dalian Customs, 60 Changjiang East Road, Dalian, Liaoning, 110060, People's Republic of China.
J Chromatogr Sci. 2023 Oct 3;61(8):790-798. doi: 10.1093/chromsci/bmac075.
Microwave-assisted dispersive liquid-liquid microextraction (MADLLME) coupled with high-performance liquid chromatography (HPLC) with diode array detector was used for the extraction and determination of three biogenic amines (BAs), including tryptamine, histamine and phenylethylamine in beverages (beer, cherry juice and white spirit). Compared with solid-phase extraction, solid-phase microextraction and liquid-phase microextraction, which is more solvent use with lower extraction efficiency, this MADLLME method obviously shortened analytical time, the rapid heating of aqueous samples with non-ionizing electromagnetic radiation, a lower solvent use and enhanced extraction efficiency. Because of good extraction for three BAs, [3C6PC14][FeCl4] was used as an extraction solvent. We showed a tunable selectivity of magnetic ionic liquids (MILs) toward extracting BAs by changing anion or cation due to the modification of the interaction between the MIL and the BAs. Extraction conditions including the type and volume of extraction solvent, microwave power, microwave-assisted extraction time, sample pH, disperser and interference experiment were investigated. Under the optimal conditions, a good linear relationship was found in the concentration range of 100-2,000 ng mL-1 for three BAs with correlation coefficient (R2) of 0.995-0.999. The limit of detections (S/N = 3) and limit of quantitations (S/N = 10) were in the range of 3.46-4.96 ng mL-1 and 10.44-14.88 ng mL-1, respectively. The recoveries of three targets were in the range of 84.3-108.5%, and the relative standard deviations based on the peak areas for six replicate analyses of beverages spiked with 10, 50 and 100 ng mL-1 of each biogenic amine were lower than 7.9%. This method has also been successfully applied to analyze the real samples at three different spiked concentrations, and excellent results have been obtained.
微波辅助分散液液微萃取（MADLLME）结合配有二极管阵列检测器的高效液相色谱（HPLC）用于饮料（啤酒、樱桃汁和白酒）中三种生物胺（BAs）的萃取和测定，这三种生物胺包括色胺、组胺和苯乙胺。与固相萃取、固相微萃取以及液相微萃取相比（液相微萃取使用更多溶剂且萃取效率较低），这种MADLLME方法明显缩短了分析时间，利用非电离电磁辐射对水性样品进行快速加热，减少了溶剂使用量并提高了萃取效率。由于对三种生物胺具有良好的萃取效果，[3C6PC14][FeCl4]被用作萃取溶剂。我们发现，通过改变阴离子或阳离子，磁性离子液体（MILs）对生物胺的萃取具有可调节的选择性，这是由于MIL与生物胺之间相互作用的改变所致。研究了萃取条件，包括萃取溶剂的类型和体积、微波功率、微波辅助萃取时间、样品pH值、分散剂以及干扰实验。在最佳条件下，三种生物胺在100 - 2000 ng mL-1浓度范围内呈现良好的线性关系，相关系数（R2）为0.995 - 0.999。检测限（S/N = 3）和定量限（S/N = 10）分别在3.46 - 4.96 ng mL-1和10.44 - 14.88 ng mL-1范围内。三种目标物的回收率在84.3 - 108.5%范围内，对于添加了10、50和100 ng mL-1每种生物胺的饮料进行六次重复分析，基于峰面积的相对标准偏差低于7.9%。该方法还成功应用于分析三种不同加标浓度的实际样品，并获得了优异的结果。
