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投稿时间:2020-08-05
投稿时间:2020-08-05
中文摘要: 建立高效液相色谱-串联质谱技术(high performance liquid chromatography-tandem mass spectrometry,HPLCMS-MS)同时测定动物源性食品中肾上腺素和多巴胺含量的检测方法。动物源性食品试样用磷酸盐缓冲液提取,弱阴离子交换固相萃取小柱净化;Thermo Hypersil GOLD C18色谱柱(4.6 mm×50 mm,1.9 μm)分离,流动相分别为0.1%甲酸-水和乙腈;采用HPLC-MS-MS法,正离子模式扫描、电喷雾电离(ESI+)、多反应监测(multiple reaction monitoring,MRM),内标法定量。结果表明:肾上腺素和多巴胺在10 ng/mL~500 ng/mL范围内线性良好,相关系数大于0.999;畜肉及其制品中定量限为 25 μg/kg,蛋、奶及蛋奶制品中定量限为 50 μg/kg;添加量为 25 μg/kg~500 μg/kg 的肾上腺素和多巴胺的回收率均在81.7%~113.7%之间,方法的精密度在1.0%~10.4%之间(n=6)。该方法能有效的降低前处理中的基质效应,为动物源性食品中肾上腺素和多巴胺的检测提供可靠的方法。
Abstract:A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS-MS)method was developed for the simultaneous determination of epinephrine and dopamine in animal-derived foods.Animal-derived food samples were extracted with phosphate buffer and purified by weak anion exchange solid phase extraction column;the separation was performed on a Thermo Hypersil GOLD C18column(4.6mm×50mm,1.9 μm) with a mobile phase of 0.1% formic acid water and acetonitrile;HPLC-MS-MS method,positive ion mode scanning,electrospray ionization (ESI+),multiple reaction monitoring (MRM),and internal standard method were used to realize quantitative analysis.The results showed that:epinephrine and dopamine had good linearity in the range of 10 ng/mL-500 ng/mL,the correlation coefficient was greater than 0.999;the limit of quantitation in meat and meat products was 25 μg/kg,the limit of quantification of egg,milk and egg milk products was 50 μg/kg;the recoveries of epinephrine and dopamine in the range of 25 μg/kg-500 μg/kg were 81.7%-113.7%,the precision of the method was between 1.0%-10.4%(n=6).The method can effectively reduce the matrix effect in the pretreatmentand provide a reliable method for the determination of epinephrine and dopamine in animal derived food.
keywords: epinephrine dopamine animal-derived foods solid phase extraction internal standard method high performance liquid chromatography-tandem mass spectrometry(HPLC-MS-MS)
文章编号:202113023 中图分类号: 文献标志码:
基金项目:国家重点研发计划(2018YFC1602302);北京市科技计划(Z181100009318011)
Author Name | Affiliation |
ZHANG Shan,ZHOU Rui-ze,ZHANG Wen-chao,PEI Fan,SHI Hai-liang | Beijing Municipal Center for Food Safety Monitoring and Risk Assessment,Beijing 100094,China |
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