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UPLC-MS/MS法测定猪肉和牛肉中褪黑素残留量OA

Determination of melatonin residues in pork and beef by UPLC-MS/MS

中文摘要英文摘要

为了监控猪肉和牛肉中的褪黑素残留量,建立超高效液相色谱-串联质谱法(UPLC-MS/MS).样品经过氨水(体积分数1%)-乙酸乙酯溶液提取,正己烷脱脂净化,采用Atlantis T3色谱柱(2.1 mm×50 mm,1.8 μm)分离,以甲酸(体积分数0.1%)溶液和乙腈为流动相进行洗脱,目标化合物在4 min内得到良好分离;在电喷雾离子源正离子模式(ESI+)下电离,多反应监测(MRM)模式检测.结果表明,褪黑素的质量浓度在1.00~100 μg/L范围内线性关系良好,相关系数均≥0.99,检出限为0.5 μg/kg,定量限为1.0 μg/kg;检测平均加标回收率为64.6%~91.5%,相对标准偏差为0.85%~6.70%.研究为畜肉产品的安全监管提供技术支持.

To monitor the residue levels of melatonin in pork and beef,an analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.Samples were extracted with 1%(V/V)ammonia water in ethyl acetate and purified by n-hexane degreasing.Chromatographic separation was performed on a Atlantis T3 column(2.1 mm×50 mm,1.8 μm)using a mobile phase consisting of 0.1%(V/V)formic acid in water and acetonitrile,achieving baseline separation of the target compound within 4 min.Detection was carried out using electrospray ionization in positive ion mode(ESI+)and multiple reaction monitoring(MRM).The results demonstrated that melatonin exhibited good linearity in the concentration range of 1.00~100 μg/L,with correlation coefficients≥0.99.The limit of detection was 0.5 μg/kg and the limit of quantification was 1.0 μg/kg.The average recoveries at spiked levels ranged from 64.6%to 91.5%,with relative standard deviations between 0.85%and 6.70%.This study provides technical support for the safety monitoring of livestock meat products.

秦宇;陈晶

上海市质量监督检验技术研究院有限公司,上海 200233||华东理工大学 生物工程学院,上海 200237上海农林职业技术学院 生物医药与健康系,上海 201699

农业科技

超高效液相色谱-串联质谱褪黑素残留猪肉牛肉

ultra-high performance liquid chromatography-tandem mass spectrometrymelatonin residuesporkbeef

《包装与食品机械》 2026 (4)

89-95,7

上海市科学技术委员会项目(24142200900)

10.3969/j.issn.1005-1295.2026.04.009

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