摘要
采用超高效液相色谱-串联质谱法建立了检测牛奶中糠氨酸含量的分析方法。试样经10.6 mol/L盐酸水解,纯水稀释后,糠氨酸在C18色谱柱上以0.1%甲酸水溶液和乙腈为流动相,进行液相色谱分离;质谱检测采用电喷雾正离子化模式和多反应监测模式(MRM)。结果表明,糠氨酸在0.01~0.5 mg/L范围内线性关系良好,相关系数(R2)为0.9996,定量限(LOQ)为0.5 mg/100 g蛋白。在生牛乳空白样品中添加浓度为10,100,300 mg/100 g蛋白时,糠氨酸的平均回收率为93.1%~95.7%,相对标准偏差(RSDs)为1.2%~1.7%(n=6)。
A method for the determination of furosine in milk by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The samples were hydrolysed by 10.6 mol/L HCl and then diluted by water,furosine was separated on a Waters BEH C18 column with gradient elution with the mobile phase of 0.1%formic acid and acetonitrile,and finally detected by positive electrospray ionization(ESI+)-MS/MS in multiple reaction monitoring(MRM)mode.The results showed the linearity of furosine was good in the concentration range of 0.01-0.5 mg/L,and the correlation coefficient(R2)was 0.9996.The limit of quantification(LOQ)of furosine was 0.5 mg/100 g protein.At the spiked levels of 10,100 and 300 mg/100 g protein in the blank raw milk samples,the mean recoveries of furosine were 93.1%-95.7%,and the relative standard deviations(RSDs)of furosine were 1.2%-1.7%(n=6).
作者
户江涛
HU Jiangtao(Food Quality Supervision and Testing Center(Jiamusi),Ministry of Agriculture and Rural Affairs,Testing and Analysis Center of Heilongjiang Academy of Land Reclamation Sciences,Jiamusi 154007)
出处
《分析试验室》
CAS
CSCD
北大核心
2020年第3期346-349,共4页
Chinese Journal of Analysis Laboratory
