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建立了超高效液相色谱-三重四级杆/线性离子阱质谱(QTRAP-UPLC-MS/MS)测定水产品中辐照相关的多种氨基酸及同分异构体的分析方法,并进一步建立了辐照水产品快速检测方法。水产品通过0.1%甲酸溶液直接超声快速提取氨基酸及同分异构体,采用Waters Acquity UPLC BEH C_(18)柱,0.1%甲酸溶液和甲醇为流动相进行梯度洗脱,正离子(ESI+)模式可快速有效分离及准确测定辐照水产品中的对酪氨酸(p-Tyrosine)、苯丙氨酸(Phenylalanine)及其辐照特异性产物间酪氨酸(m-Tyrosine)和邻酪氨酸(o-Tyrosine)的含量,MRM-IDA-EPI模式对辐照特异性产物二次定性。结果表明:在10~500μg/L范围内,所测氨基酸及同分异构体的线性相关系数在0.9987~0.9995之间,回收率在76.8%~97.6%,相对标准偏差小于8.5%。在M RM-IDA-EPI模式监测下,可准确对辐照水产品中的特异性产物m-Tyrosine和o-Tyrosine进行二次定性。本方法适用于含蛋白质辐照水产品的快速准确检测,尤其是脂肪含量低且无法分离出硅酸盐物质的水产品,解决了辐照水产品的检测及食品安全监控问题。
A method for the determination of various irradiation-related amino acids and their isomers in aquatic products by ultra performance liquid chromatography-triple quadrupole / linear ion trap mass spectrometry (QTRAP-UPLC-MS / MS) was established and further established The rapid detection of irradiated aquatic products. Aquatic products were rapidly extracted by 0.1% formic acid solution. The mobile phases were eluted with a Waters Acquity UPLC BEH C 18 column, 0.1% formic acid and methanol. The positive ion (ESI +) mode Rapid and effective separation and accurate determination of irradiated aquatic products on the tyrosine (p-Tyrosine), phenylalanine (Phenylalanine) and its radiation-specific product between the tyrosine (tyrosine) and the adjacent tyramine Acid (o-Tyrosine) content, MRM-IDA-EPI mode secondary characterization of irradiation-specific products. The results showed that the linear correlation coefficients of amino acid and its isomers ranged from 0.9987 to 0.9995 and the recoveries ranged from 76.8% to 97.6% and the relative standard deviations were less than 8.5% in the range of 10-500 μg / L. M-Tyrosine and o-Tyrosine, specific products of irradiated aquatic products, can be accurately characterized with M RM-IDA-EPI mode monitoring. The method is suitable for the rapid and accurate detection of protein-irradiated aquatic products, especially the aquatic products with low fat content and unable to separate silicate substances, and solves the problems of radiation aquatic product testing and food safety monitoring.