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[目的]建立人尿中的三聚氰胺液相色谱-串联质谱测定法。[方法]尿样经0.2 mol/L盐酸酸化,乙腈超声提取,MCX固相萃取柱净化及浓缩后,10μL进样,并用液相色谱-串联质谱仪进行检测,检测的色谱条件为:色谱柱为CAPCELL PAK CR SCX∶C18=1∶4,流动相为10 mmol/L的乙酸铵-乙腈-0.1%甲酸混和溶液(体积分数40∶50∶10),柱温为30℃,流速为0.2 m L/min。[结果]三聚氰胺的保留时间3.95min,三聚氰胺在5~200μg/L的浓度范围内呈线性关系,R2为0.999 8。浓度在10、50、100μg/L时,回收率在96.7%~97.2%范围内,相对标准偏差≤5.16%,最低检出限为0.6μg/L,最低定量限为2μg/L。[结论]该方法前处理简便,灵敏度高,适合用来检测人尿液中三聚氰胺。
[Objective] To establish a method for the determination of melamine in human urine by liquid chromatography-tandem mass spectrometry. [Method] The urine sample was extracted with 10 mol hydrochloric acid, 0.2 mmol / L hydrochloric acid, acetonitrile, and purified by MCX solid phase extraction. The chromatographic conditions were as follows: The mixture of ammonium acetate-acetonitrile-0.1% formic acid (volume fraction 40:50:10) with CAPCELL PAK CR SCX: C18 = 1: 4 and mobile phase of 10 mmol / L was used. The column temperature was 30 ℃ and the flow rate was 0.2 m L / min. [Result] The retention time of melamine was 3.95min, the linear relationship of melamine in the concentration range of 5 ~ 200μg / L, R2 was 0.999 8. The recoveries ranged from 96.7% to 97.2% when the concentration was 10,50,100μg / L, the relative standard deviation was less than or equal to 5.1%, the lowest detection limit was 0.6μg / L and the lowest limit of quantification was 2μg / L. [Conclusion] The method has simple pre-treatment and high sensitivity and is suitable for detecting melamine in human urine.