摘要
建立了固相萃取-超高效液相色谱串联质谱测定海水及沉积物中三聚氰胺的方法。水样过滤后经Bond ElutRlexaTMPCX固相萃取柱净化,富集。沉积物样品用1%的三氯乙酸提取,经Bond ElutPlexaTMPCX柱净化,以乙腈和含有0.1%甲酸的5 mmol.L^-1乙酸铵为流动相,用超高效液相色谱串联质谱测定,沉积物中三聚氰胺的检出限为0.5μg.kg^-1,添加量为0.5-5.0μg.kg^-1水平时,平均回收率均大于70%,相对标准偏差均小于12%;海水中三聚氰胺的检出限为1.0 ng.L^-1,添加量为1.0-10.0 ng.L^-1水平时,平均回收率均大于75%,相对标准偏差均小于10%。
A method for determination of melamine in seawater and sediments was established by UPLC-MS/MS. Water samples were filtered, and extracted by Bond Elut Plexa^TM PCX cartridges. Sediment samples were extracted with 1 M trichloroacetic acid solution, and then cleaned with Bond Elut PlexaTM PCX cartridges. The analyte was separated with 5 mmol· L^-1 ammonium acetate （containing 0. 1% formic acid）-acetonitrile as mobile phase, and determined by UPLC-MS/MS. The limit of detection in sediments is 0.5 μg ·kg-1. When spiked 0.5-5.0 μg · kg^-1 in sediments, the mean recovery is over 70%, and the RSDs are less than 12%. The limit of detection in seawater is 1. 0 ng · L^-1. When spiked 1.0-10.0 ng · L^-1 in seawater, the mean recovery is over 75%, and the RSDs are less than 10%.
出处
《质谱学报》
EI
CAS
CSCD
2009年第2期70-73,共4页
Journal of Chinese Mass Spectrometry Society
