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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 被引量:7

Determination of Melamine Residues in Feed by UPLC-MS-MS
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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%.
出处 《食品工业》 北大核心 2009年第5期58-60,共3页 The Food Industry
关键词 超高液相-串联质谱法 内标法 三聚氰胺 饲料 UPLC-MS-MS internal method melamine feed
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