超高效液相色谱-串联质谱内标法测定饲料中三聚氰胺含量  

Determination of Melamine Residues in Feed by UPLC-MS-MS

作　　者：付登洲[1] 杨雪娇[1] 黄伟[1] 吕维佳[1] 

机构地区：[1]东莞出入境检验检疫局,东莞523072

出　　处：《食品工业》2009年第5期58-60,共3页The Food Industry

摘　　要：应用超高效液相色谱-串联质谱内标法测定饲料中三聚氰胺含量。样品用1%三氯乙酸溶液提取,高速离心,经固相萃取柱净化后,超高液相-串联质谱仪测定,内标法定量。采用电喷雾(ESI)正离子扫描模式、多反应监测(MRM)方式监测。三聚氰胺检出限0.5ng/mL,线性方程的相关系数r>0.99,在添加浓度(2～10)μg/kg范围内,三聚氰胺的回收率为84%～101.4%,相对标准偏差(RSD)小于9.6%。Ultra performance liquid chromatography tandem mass spectrometry （UPLC-MS-MS） method was applied to the determination of residual amounts of melamine. Test sample was extracted with 1% trichloroacetic acid solution. The extract was centrifuged before it was purified with solid phase extraction. The supernatant was determined by UPLC-MS-MS, internal method for quantification. Identification was performed by multiple reaction monitoring（MRM）, and electrospray ionization was positive mode. The limit of detection for melamine was 0.5 ng/mL, correlation coefficient of linear regression equations was above 0.99 and the recoveries were in the range of 84%-101.4%, at spiked levels of （2-10） μg/kg. The RSD of the method was less than 9.6%.

关 键 词：超高液相-串联质谱法 内标法 三聚氰胺 饲料 

分 类 号：S816.2[农业科学—饲料科学]