摘要
建立了饲料中三聚氰胺的高效液相色谱-质谱测定方法。色谱条件：Kromasil C18柱（4.6mm×250mm，5μm），流动相：乙腈-0.1％（体积分数）甲酸（体积比5：95），流速0．4mL／min。采用正离子模式的电喷雾质谱检测，以一级质谱得到的准分子离子m／z 127作为母离子，进行碰撞诱导解离（CID）二级质谱（MS^2）分析，选择母离子和MS^2的碎片离子m／z 85、109定性确证，提取m／z 85、109、127三个离子质量色谱峰面积定量。实验优化了质谱条件。线性范围为0．01-0．5mg／L，检出限0．01mg／L（S／N=3），回收率为80％-99％。
A method for determination of melamine in feeds and food addives by liquid chromatogra-phy- mass spectrum （ LC - MS/MS） was established. The conditions of LC - MS was optimized. The sample was extracted and separated on a Kromasil -C18 column（4.6mm×250mm, 5μm） with acetonitrile -0.1% formic acid（5：95, by volume） as the mobile phase at flow rate 0.4 mL/min, and determined by （ ＋ ）ESI MS/MS. The parent ion of （ ＋ ）ESI MS was m/z 127, and it＇s daugh- ter ions of MS/MS m/z 85, 109 were selected as qualitative. The TIC of MS/MS was selected as quantitative of melamine. A linear calibration curve was obtained in the concentration range of 0.01 - 0.5 mg/L. The melamine recovery was in the range of 80% - 99% , the limit of determination was 0.01 mg/L（S/N = 3）. The method proved to be simple and accurate, and has been applied to determination of melamine in feeds and food additives.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第3期313-315,共3页
Journal of Instrumental Analysis
关键词
三聚氰胺
液相色谱-质谱
饲料
食品添加剂
melamine
liquid chromatography- mass spectrum
feeds
food additives
作者简介
黄芳（1975-），女，湖南岳阳人，高级工程师，Tel：020-37656312，E-mail：thymol206@mail.china.com
