液相色谱-串联质谱法测定饲料中16种氨基酸

Determination of 16 amino acids in feed by liquid chromatography-tandem mass spectrometry

试验旨在建立检测饲料中16种氨基酸的液相色谱-串联质谱(LC-MS)方法。采用C18反相色谱柱进行组分分离,以0.1%甲酸水和甲醇按梯度洗脱程序进行洗脱,优化色谱条件和质谱参数。结果表明,16种氨基酸在0.01~50.00μmol/L范围内线性良好,线性相关系数均大于0.9910,检出限为1~10 ng/g,定性重复性为0.02%~0.12%,定量重复性为0.11%~0.94%,回收率为97.3%~104.0%。在不同种类的样品测试中,该方法与国家标准方法的相对偏差均小于5%,结果准确可靠。试验方法检测效率高、灵敏度高、回收效果良好、定性和定量准确,能够满足饲料中16种氨基酸的常规检测。

The purpose of the experiment was to establish a liquid chromatography-tandem mass spectrometry(LC-MS)method for the detection of 16 amino acids in feed.A C18 reversed-phase chromatographic column was used for component separation,and elution was carried out with 0.1%formic acid water and methanol according to a gradient elution procedure,and the chromatographic conditions and mass spectrometry parameters were optimized.The results showed that the 16 amino acids had good linearity in the range of 0.01~50.00μmol/L,the linear correlation coefficients were all greater than 0.9910,the detection limit was 1~10 ng/g,and the qualitative repeatability was 0.02%~0.12%.The quantitative repeatability was 0.11%~0.94%,and the recovery rate was 97.3%~104.0%.In different types of sample tests,the relative deviation between this method and the national standard method is less than 5%,and the results are accurate and reliable.The method can improve detection efficiency,high sensitivity,good recovery effect,qualitative and quantitative accuracy,and can meet the routine detection of 16 amino acids in feed.