{"title":"快速LC-MS/MS定量肉类中生物胺的方法:验证及在食品安全监测中的应用。","authors":"Giulia Rampazzo, Giacomo Depau, Giampiero Pagliuca, Elisa Zironi, Andrea Serraino, Federica Savini, Teresa Gazzotti","doi":"10.3390/mps8050106","DOIUrl":null,"url":null,"abstract":"<p><p>Biogenic amines (BAs) are nitrogenous compounds naturally present in protein-rich foods, whose accumulation may indicate spoilage and pose health risks. This study presents the development and validation of a rapid LC-MS/MS method for the simultaneous quantification of six BAs-putrescine (PUT), cadaverine (CAD), histamine (HIS), tyramine (TYR), spermidine (SPD), and spermine (SPM)-in meat products, without requiring derivatisation. Sample preparation was optimized to enhance extraction efficiency and reproducibility, using 0.5 M HCl and a double-centrifugation protocol to avoid matrix interference. Chromatographic separation was optimized using a C18 column and acidified ammonium formate/acetonitrile mobile phases. The method showed good linearity (R<sup>2</sup> > 0.99), trueness between -20% and +20%, and acceptable precision (RSD<sub>r</sub> and RSD<sub>R</sub> ≤ 25%). Limits of quantification were established at 10 µg/g for all analytes. The method was applied to ten commercial meat samples, where PUT, TYR, and SPD were the most frequently detected amines. Although HIS and TYR levels were below toxicological thresholds for healthy individuals, one sample showed TYR levels potentially concerning for monoamine oxidase inhibitors -treated consumers. The Biogenic Amine Index (BAI) further supported product quality assessment, identifying early spoilage in selected cases. This method offers a rapid, robust and efficient tool for routine monitoring of BAs in meat products, supporting food safety and quality control initiatives.</p>","PeriodicalId":18715,"journal":{"name":"Methods and Protocols","volume":"8 5","pages":""},"PeriodicalIF":2.0000,"publicationDate":"2025-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12452713/pdf/","citationCount":"0","resultStr":"{\"title\":\"A Rapid LC-MS/MS Method for Quantification of Biogenic Amines in Meat: Validation and Application for Food Safety Monitoring.\",\"authors\":\"Giulia Rampazzo, Giacomo Depau, Giampiero Pagliuca, Elisa Zironi, Andrea Serraino, Federica Savini, Teresa Gazzotti\",\"doi\":\"10.3390/mps8050106\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Biogenic amines (BAs) are nitrogenous compounds naturally present in protein-rich foods, whose accumulation may indicate spoilage and pose health risks. 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Although HIS and TYR levels were below toxicological thresholds for healthy individuals, one sample showed TYR levels potentially concerning for monoamine oxidase inhibitors -treated consumers. The Biogenic Amine Index (BAI) further supported product quality assessment, identifying early spoilage in selected cases. 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引用次数: 0
摘要
生物胺(BAs)是天然存在于富含蛋白质的食物中的含氮化合物,其积累可能表明食物变质并构成健康风险。本研究提出了一种快速LC-MS/MS方法,用于同时定量肉类产品中6种bas -腐胺(PUT)、尸胺(CAD)、组胺(HIS)、酪胺(TYR)、亚精胺(SPD)和精胺(SPM),而不需要衍生化。为了提高提取效率和重现性,对样品制备进行了优化,使用0.5 M HCl和双离心方案以避免基质干扰。采用C18色谱柱和酸化甲酸铵/乙腈流动相优化分离。方法线性良好(R2为0.99),准确度在-20% ~ +20%之间,精密度可接受(RSDr和RSDr≤25%)。所有分析物的定量限均为10µg/g。该方法应用于10个商业肉类样品,其中PUT, TYR和SPD是最常检测到的胺。虽然HIS和TYR水平低于健康个体的毒理学阈值,但一个样本显示TYR水平可能与单胺氧化酶抑制剂治疗的消费者有关。生物胺指数(BAI)进一步支持产品质量评估,在选定的情况下识别早期变质。该方法为肉制品中ba的常规监测提供了一种快速、稳健和高效的工具,支持食品安全和质量控制举措。
A Rapid LC-MS/MS Method for Quantification of Biogenic Amines in Meat: Validation and Application for Food Safety Monitoring.
Biogenic amines (BAs) are nitrogenous compounds naturally present in protein-rich foods, whose accumulation may indicate spoilage and pose health risks. This study presents the development and validation of a rapid LC-MS/MS method for the simultaneous quantification of six BAs-putrescine (PUT), cadaverine (CAD), histamine (HIS), tyramine (TYR), spermidine (SPD), and spermine (SPM)-in meat products, without requiring derivatisation. Sample preparation was optimized to enhance extraction efficiency and reproducibility, using 0.5 M HCl and a double-centrifugation protocol to avoid matrix interference. Chromatographic separation was optimized using a C18 column and acidified ammonium formate/acetonitrile mobile phases. The method showed good linearity (R2 > 0.99), trueness between -20% and +20%, and acceptable precision (RSDr and RSDR ≤ 25%). Limits of quantification were established at 10 µg/g for all analytes. The method was applied to ten commercial meat samples, where PUT, TYR, and SPD were the most frequently detected amines. Although HIS and TYR levels were below toxicological thresholds for healthy individuals, one sample showed TYR levels potentially concerning for monoamine oxidase inhibitors -treated consumers. The Biogenic Amine Index (BAI) further supported product quality assessment, identifying early spoilage in selected cases. This method offers a rapid, robust and efficient tool for routine monitoring of BAs in meat products, supporting food safety and quality control initiatives.