液相色谱串联三重四极杆质谱法检测饲料三聚氰胺的研究

Rapid determination of melamine in feeds with liquid chromatography coupled to triple quadrupole mass spectrometry

使用三氯乙酸溶液沉淀样品中的蛋白并提取目标化合物,采用MCX柱净化提取物,使用CN液相色谱柱,流动相为甲醇∶5 mmol/L乙酸铵=10∶90(V/V)。电喷雾离子源(ESI)电离,多反应监测(MRM)方式对三聚氰胺作定性和定量分析。在浓度为1.0～1000.0μg/L的范围内线性良好(r>0.999)。在40.0、400.0、800.0、2000.0μg/kg添加水平下,回收率在81.2～96.7%,相对标准偏差为2.1～7.3%。检测限(S/N=5)为2.0μg/kg。

Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix. The dissociated was purified by MCX column, chromatographic conditions included a Kromasil CN column with the mobile phase of V（methanol）＋V（5mmol/Lammonium acetate）=10＋90. Qualitative and quantitative analysis of the melamine which ionized by electrospray ionization interface（ESI） was carry on through MRM mode. There was a good linear correlation in the range of 1.0-1000.0 μg/L （r〉0.999）.The recoveries ranged from 81.2% to 96.7% at the add concentration level 40.0,400.0,800.0, 2000.0 μg/kg. The RSD was between 2.1% and 7.3%.Its limit of detection was 2.0 μg/kg.