[关键词]
[摘要]
建立了同时测定酱油中8种生物胺的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品中加入1,7-庚二胺作为内标,以水稀释和氨水调节pH值后,加入乙腈进行液液萃取,盐析分层,萃取液经QuEChERS净化,调整酸度、浓缩、复溶后,以UPLC-MS/MS分离测定,内标法定量。在优化条件下,8种待测物在5.0 μg/L ~ 500 μg/L浓度范围内线性关系良好,相关系数均大于0.998;方法检出限为30 μg/kg ~ 60 μg/kg,方法定量限为120 μg/kg ~ 250 μg/kg;在酱油样品中进行2个水平的添加实验(n=6),平均回收率为83.7%~110%,相对标准偏差为3.8%~11.5%。实际酱油样品检测结果显示,酱油中酪胺和苯乙胺的含量最高。本方法准确、灵敏、快速,适用于酱油中8种生物胺的同时测定。
[Key word]
[Abstract]
An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous determination of eight biogenic amines in soybean sauce. 1, 7-Heptanediamine was added to the samples and used as the internal standard. Samples were diluted in water and pH values were adjusted using ammonia water. The sample solution was then extracted by acetonitrile using liquid-liquid extraction and salting out methods. The extract was subsequently purified by using Quick Easy Cheap Effective Rugged Safe (QuEChERS). After the acidity of the extract was adjusted and the solution was concentrated and reconstituted, all samples were separated and measured by using UPLC-MS/MS and quantitatively AND analyzed using an internal standard method. Under the optimized conditions, the calibration curves of eight analytes showed a good linearity over a concentration range of 5.0~500 μg/L, with coefficients of determination (R2) greater than 0.998. The limits of detection (LODs) and the limits of quantitation (LOQs) of the method were in the range of 30~60 μg/kg and 120~250 μg/kg, respectively. The spike and recovery experiments at two levels of concentration in soybean sauce samples (n = 6) were performed. The average recoveries were found to be between 83.7% and 110%, with relative standard deviation (RSD) values of 3.8~11.5%. The detection results on the actual soybean sauce samples revealed that the content of tyramine and phenylethylamine were the highest in the samples. The developed method is accurate, sensitive, rapid, and suitable for the simultaneous determination of eight biogenic amines in soybean sauce.
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