高效液相色谱-串联质谱法测定饲料中三聚氰胺

本研究建立了高效液相色谱-串联质谱(LC-MS/MS)测定饲料中三聚氰胺含量的方法。饲料用三氯乙酸和乙酸铅溶液提取,再经PCX固相萃取柱净化,HILIC色谱柱分离、电喷雾离子化(ESI^+)和选择反应监测(SRM)方式采集,并以^(15)N_3-三聚氰胺为同位素内标定量。该方法的检出限为1 μg/kg;三聚氰胺的测定在1～50ng/mL时具有良好的线性关系;配合饲料、浓缩饲料、预混饲料中的平均回收率分别为97.5%、98.9%和98.0%,平均变异系数分别为4.3%、4.1%和4.3%。通过与外标法比较,该方法定量准确可靠,更加适合用作饲料中三聚氰胺的定量测定。

A high performance liquid chromatography-tandem mass spectrometry method （LC-MS/MS） has been established for the determination of melamine in animal feed.The samples were extracted with the solution of trichloroacetic acid and lead acetate ,cleaned by PCX SPE cartridges and separated through a HILIC column.Mass spectrometry eondition：eleetrospray ionization （ESI＋）and selected reaction monitoring （SRM）mode.The detection used lSN3-melamine as the isotopic internal standard.The limit of detection （LOD）of the method was 1 μg/kg.The calibration curve had good linear within the range of ribavirin concentration from 1 ng/mL to 50 ng/mL.The mean recovery of melamine in formula feed, concentrated feed and premix was 97.5 %,98.9 % and 98.0 %,and the mean RSD was 4.3 %,4.1% and 4.3 %,respectively. Compared with the external standard method, the method was accurate and reliable in quantification, and it was more propitious to be used for the quantitative determination of melamine in feed.