超高效液相色谱-串联质谱测定海水及沉积物中三聚氰胺

Determination of Melamine in Seawater and Sediments by UPLC-MS/MS

  • 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 Elut Plexa TM PCX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 Elut Plexa TM PCX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0.5 μg•kg-1, 添加量为0.5~5.0 μg•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%。

     

    Abstract: 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% trichloroacetic acid solution, and then cleaned with Bond Elut Plexa TM 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%.

     

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