Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário, Seção Laboratorial Avançada de São José (SLAV/SC/LANAGRO/RS), São José, SC 88102-600, Brazil; Instituto Catarinense de Sanidade Agropecuária (ICASA), Florianópolis, SC 88034-001, Brazil; Universidade Federal de Santa Catarina (UFSC), Programa de Pós-graduação em Ciência de Alimentos, Florianópolis, SC 88034-001, Brazil.
Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Nacional Agropecuário, Seção Laboratorial Avançada de São José (SLAV/SC/LANAGRO/RS), São José, SC 88102-600, Brazil.
Talanta. 2018 Feb 1;178:1053-1066. doi: 10.1016/j.talanta.2017.08.081. Epub 2017 Aug 30.
This paper describes an innovative fast and multipurpose method for the chemical inspection of meat and fish products by liquid chromatography-tandem mass spectrometry. Solid-liquid extraction and low temperature partitioning were applied to 17 analytes, which included large bacteriocins (3.5kDa) and small molecules (organic acids, heterocyclic compounds, polyene macrolides, alkyl esters of the p-hydroxybenzoic acid, aromatic, and aliphatic biogenic amines and polyamines). Chromatographic separation was achieved in 10min, using stationary phase of di-isopropyl-3-aminopropyl silane bound to hydroxylated silica. Method validation was in accordance to Commission Decision 657/2002/CE. Linear ranges were among 1.25-10.0mgkg (natamycin and parabens), 2.50-10.0mgkg (sorbate and nisin), 25.0-200mgkg (biogenic amines, hexamethylenetetramine, benzoic and lactic acids), and 50.0-400mgkg (citric acid). Expanded measurement uncertainty (U) was estimated by single laboratory validation combined to modeling in two calculation approaches: internal (U = 5%) and external standardization (U = 24%). Method applicability was checked on 89 real samples among raw, cooked, dry fermented and cured products, yielding acceptable recoveries. Many regulatory issues were revealed, corroborating the need for enhancement of the current analytical methods. This simple execution method dispenses the use of additional procedures of extraction and, therefore, reduces costs over time. It is suitable for routine analysis as a screening or confirmatory tool for both qualitative and quantitative results, replacing many time consuming analytical procedures.
本文描述了一种新颖的快速多用途方法,用于通过液相色谱-串联质谱法对肉类和鱼类产品进行化学检查。固相萃取和低温分配应用于 17 种分析物,包括大型细菌素(3.5kDa)和小分子(有机酸、杂环化合物、多烯大环内酯、对羟基苯甲酸的烷基酯、芳香族和脂肪族生物胺和多胺)。使用键合有羟基化硅胶的二异丙基-3-氨丙基硅烷作为固定相,在 10min 内实现了色谱分离。方法验证符合委员会决定 657/2002/CE。线性范围在 1.25-10.0mgkg(纳他霉素和对羟基苯甲酸酯)、2.50-10.0mgkg(山梨酸钾和乳链菌肽)、25.0-200mgkg(生物胺、六亚甲基四胺、苯甲酸和乳酸)和 50.0-400mgkg(柠檬酸)之间。通过单实验室验证结合两种计算方法(内部标准化(U = 5%)和外部标准化(U = 24%))来估计扩展的测量不确定度(U)。方法适用性通过在生、熟、干发酵和腌制产品中的 89 个实际样品中进行检查,得到了可接受的回收率。发现了许多监管问题,证实需要加强当前的分析方法。这种简单的执行方法无需使用额外的提取程序,因此随着时间的推移降低了成本。它适合作为筛选或定性和定量结果的确证工具进行常规分析,可替代许多耗时的分析程序。