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Development of a SALLE-HPLC-FLD Analytical Method for the Simultaneous Determination of Ten Biogenic Amines in Cheese
Food Analytical Methods ( IF 2.6 ) Pub Date : 2020-02-18 , DOI: 10.1007/s12161-020-01730-6
Rui Miguel Ramos , Pedro Francisco Brandão , José António Rodrigues

In this work, a new methodology for the determination of biogenic amines in cheese is presented, which includes an innovative sample preparation approach based on salting-out assisted liquid-liquid extraction (SALLE). The method features a pre-extraction of the soluble biogenic amines with hydrochloric acid, a derivatization with dansyl chloride, the use of the salting-out effect, and the analysis of the derivatized biogenic amines using high-performance liquid chromatography with fluorescence detection. Several extraction parameters were studied and optimized, such as the HCl extraction time, concentration of the derivatization reagent and influence of the medium’s pH, among others. For the considered biogenic amines, the developed method exhibits adequate limits of detection (0.015 to 1.77 mg L−1) and quantification (0.050 to 5.91 mg L−1) and average recoveries between 94 and 110%, with the highest determined amounts found for putrescine, dimethylamine and histamine. Furthermore, mass spectrometry studies identified and confirmed the presence of several biogenic amines in the samples. SALLE stands as a good alternative to existing methods, since it simplifies the sample preparation step, while improving the overall selectivity of the process. It may also be adopted for the determination of biogenic amines in different solid samples besides cheese, such as meat, fish or other food products.



中文翻译:

同时测定奶酪中十种生物胺的SALLE-HPLC-FLD分析方法的建立

在这项工作中,提出了一种测定奶酪中生物胺的新方法,其中包括基于盐析辅助液液萃取(SALLE)的创新样品制备方法。该方法具有可溶的生物胺与盐酸的预萃取,丹磺酰氯的衍生化,利用盐析作用以及使用具有荧光检测功能的高效液相色谱法对衍生的生物胺的分析。研究和优化了几种萃取参数,例如HCl萃取时间,衍生化试剂的浓度和介质pH值的影响等。对于所考虑的生物胺,开发的方法具有足够的检测限(0.015至1.77 mg L -1)和定量分析(0.050至5.91 mg L -1),平均回收率在94%至110%之间,腐胺,二甲胺和组胺的最高测定量。此外,质谱研究确定并确认了样品中存在几种生物胺。SALLE可以替代现有方法,因为它简化了样品制备步骤,同时提高了过程的整体选择性。它也可用于测定奶酪,肉类,鱼类或其他食品等不同固体样品中的生物胺。

更新日期:2020-04-21
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