摘要
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 credible QTRAP-UPLC-MS/MS method for determination of p-Tyrosine,m-Tyrosine,oTyrosine and Phenylalanine was established to identify the irradiated seafood. The optimum procedure employed a simple extraction by 0. 1% formic acid. The separation was achieved on a Waters Acquity UPLC BEH C_（18）（ 100 mm × 2. 1 mm,1. 7 μm） column with mobile phase of methanol and 0. 1%（ V/V）formic acid in Milli-Q water with gradient pump. The p-Tyrosine,Phenylalanine and m-Tyrosine o-Tyrosine as markers of irradiated seafood were analyzed by positive electrospray ionization（ ESI＋） and MRM-IDAEPI mode. The determination coefficients of the developed linear equations of these analytes were in the ranges of 0. 9987 ~ 0. 9995,and the recoveries of addition standard were within76. 8% ~ 97. 6% with RSD 8. 5%. Using the MRM-IDA-EPI mode,m-Tyrosine and o-Tyrosine as markers were precisely detected to identify irradiated seafood. This established method is rapid and accurate,and meet the requirement for irradiated protein-rich seafood identification especially for the seafood without lipid and silicate minerals.
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第5期561-566,共6页
Chinese Journal of Analysis Laboratory
基金
浙江省自然科学基金项目(LQ15c200005)
浙江省公益技术研究农业项目(2015C32101)
浙江省科技计划项目(2016C37041)资助
