采用气相色谱-稳定同位素比值质谱(Gas chromatography-stable isotope ratio mass spectrometry,GC-IRMS)技术测定三文鱼中16种氨基酸碳同位素δ13C值分布.以16种特征氨基酸为溯源分析对象,首先采用盐酸水解蛋白,再进行甲酯和乙酰化衍生反应,生成的衍生物用35％苯基-甲基聚硅氧烷色谱柱分离.在优化的GC-IRMS试验参数下,16种氨基酸方法检出限为50 mg/kg,质控品谷氨基酸在不同批次间标准偏差为0.84％.经对来自挪威、法罗群岛、澳大利亚、智利、美国、新西兰这6个产地的三文鱼进行测定,测得三文鱼δ13C值在-3.116％至-0.165％之间,标准偏差(n=5)≤4.2％.通过获得不同产地三文鱼中16种特征功能性氨基酸指纹图谱,分析了三文鱼中不同特征氨基酸功能成分间δ13C值的相关性,并对每种氨基酸对产地、养殖方式溯源因子鉴定的贡献进行了分析.在统计分析的基础上,完成不同产地、不同生长方式三文鱼的溯源鉴定模型.对实际样品进行测定,证明三文鱼体内蛋白氨基酸成分可作为特征指标,可用于对三文鱼进行产地、养殖方式进行溯源鉴别,测定结果可靠.
Traceability of Salmon from Different Origins Using Stable Isotope Fingerprinting Based on Functional Amino Acid Profiling Factors
The gas chromatography-stable isotope ratio mass spectrometry(GC-IRMS)was used to determine the δ13C value distribution of 16 amino acids in salmon.16 characteristic amino acids were used as the traceability analysis target,the protein was hydrolyzed with hydrochloric acid,and then subjected to methylation and acetylation derivative reactions,the generated derivatives were separated on a 35％phenyl-methylpolysiloxane column.Under the optimized experimental parameters of GC-IRMS,the detection limits of 16 amino acids method was 50 mg/kg,and the standard deviation of the glutamic acid in the quality control between different batches was 0.84％.After measuring salmon from six origins including Norway,the Faroe Islands,Australia,Chile,America and New Zealand,it was found that the δ13C value of salmon samples ranged from-3.116％to-0.165％,with a standard deviation(n=5)of ≤4.2％.The fingerprint maps of 16 characteristic functional amino acid were obtained from salmon from different origins,the correlation between δ13C values of different functional components of characteristic amino acids in salmon was analyzed,and the contribution of each amino acid to the identification of origin and culture method traceability factors was analyzed.Based on statistical analysis,a traceability identification model for salmon from different origins and growth methods was established.The measurement of actual samples showed that the amino acid composition in salmon proteins can serve as a characteristic indicator for the traceability and identification of salmon origin and farming methods,these measurement results are reliable.
characteristic amino acidsgas chromatography-stable isotope mass spectroscopyorigin traceabilitysalmon
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