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Solventless separation of underivatized biogenic amines by sequential injection chromatography
Microchemical Journal ( IF 4.9 ) Pub Date : 2020-07-01 , DOI: 10.1016/j.microc.2020.104839
Mariana R. Gama , Fábio R.P. Rocha

Abstract Biogenic amines (BA) are markers of food freshness and indicators of inadequate food processing and storage conditions. Because BA determination is important for food quality evaluation, and considering the relatively complex analytical procedures available, new approaches are required for their determination. In this work, an environmentally friendly analytical procedure is proposed for BA determination in cheese, involving separation by sequential injection chromatography without organic solvents or chemical derivatization of the analytes. Sample preparation step was carried out by acid protein precipitation and low-temperature partition with a reduced volume of organic solvent (500 µL of acetonitrile). Because of the previously mentioned characteristics, an analytical eco-scale = 91 was achieved. Histamine, tyramine, and tryptamine were separated in a cyanopropyl monolithic column in the isocratic elution mode, with 3.0 mmol L−1 phosphoric acid aqueous solution as mobile phase. The analytes were quantified from their intrinsic absorption at 210 nm. The analysis time was less than 3 min, with good chromatographic efficiency (N ≥ 75000 plates m−1). For the three analytes, LOD within 0.05–0.10 mg kg−1, LOQ within 0.14–0.30 mg kg−1, and linear response ranges up to 10 mg kg−1 (histamine and tyramine) and 15 mg kg−1 (tryptamine) were achieved with good precision (CV = 3.0%, n = 12). The proposed procedure was successfully applied to the determination of tyramine in cheese samples, with recoveries in the 81–128% range.

中文翻译:

通过顺序注射色谱法对​​未衍生化的生物胺进行无溶剂分离

摘要 生物胺 (BA) 是食品新鲜度的标志,也是食品加工和储存条件不足的指标。由于 BA 测定对于食品质量评估很重要,并且考虑到可用的相对复杂的分析程序,因此需要新的方法来测定它们。在这项工作中,提出了一种环境友好的分析程序来测定奶酪中的 BA,包括通过连续注射色谱法进行分离,无需有机溶剂或分析物的化学衍生化。样品制备步骤通过酸性蛋白质沉淀和低温分配进行,减少有机溶剂(500 µL 乙腈)的体积。由于前面提到的特征,实现了分析生态尺度 = 91。组胺、酪胺、和色胺在氰丙基整体柱中以等度洗脱模式分离,以3.0 mmol L-1磷酸水溶液为流动相。分析物通过其在 210 nm 处的固有吸收进行量化。分析时间小于 3 分钟,具有良好的色谱效率(N ≥ 75000 板 m-1)。对于三种分析物,LOD 在 0.05-0.10 mg kg-1 内,LOQ 在 0.14-0.30 mg kg-1 内,线性响应范围高达 10 mg kg-1(组胺和酪胺)和 15 mg kg-1(色胺)达到了良好的精度(CV = 3.0%,n = 12)。所提出的程序已成功应用于奶酪样品中酪胺的测定,回收率在 81-128% 范围内。分析物通过其在 210 nm 处的固有吸收进行量化。分析时间小于 3 分钟,具有良好的色谱效率(N ≥ 75000 板 m-1)。对于三种分析物,LOD 在 0.05-0.10 mg kg-1 内,LOQ 在 0.14-0.30 mg kg-1 内,线性响应范围高达 10 mg kg-1(组胺和酪胺)和 15 mg kg-1(色胺)达到了良好的精度(CV = 3.0%,n = 12)。所提出的程序已成功应用于奶酪样品中酪胺的测定,回收率在 81-128% 范围内。分析物通过其在 210 nm 处的固有吸收进行量化。分析时间小于 3 分钟,具有良好的色谱效率(N ≥ 75000 板 m-1)。对于三种分析物,LOD 在 0.05-0.10 mg kg-1 内,LOQ 在 0.14-0.30 mg kg-1 内,线性响应范围高达 10 mg kg-1(组胺和酪胺)和 15 mg kg-1(色胺)达到了良好的精度(CV = 3.0%,n = 12)。所提出的程序已成功应用于奶酪样品中酪胺的测定,回收率在 81-128% 范围内。线性响应范围高达 10 mg kg-1(组胺和酪胺)和 15 mg kg-1(色胺),具有良好的精度(CV = 3.0%,n = 12)。所提出的程序已成功应用于奶酪样品中酪胺的测定,回收率在 81-128% 范围内。线性响应范围高达 10 mg kg-1(组胺和酪胺)和 15 mg kg-1(色胺),具有良好的精度(CV = 3.0%,n = 12)。所提出的程序已成功应用于奶酪样品中酪胺的测定,回收率在 81-128% 范围内。
更新日期:2020-07-01
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