中文摘要：

[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。

英文摘要：

[ Objective ] To establish a method for melamine determination in human urine by liquid chromatography- tandem mass spectrometry （LC-MS/MS）. [ Methods ] Urine samples were acidized with 0.2 mol/L hydrochloric acid, extracted in acetonitrile solution assisted with ultrasound, purified and concentrated using MCX solid phase extraction （SPE） column, and detected by LC-MS/MS in a 10μL sample injection. The chromatographic conditions were as follows： Chromatographic column was CAPCELL PAK C R （SCX ： C 18 = 1 ： 4）; Mobile phase was a mixed solution （10 mmol/L） containing ammonium acetate, acetonitrile, and 0.1% formic acid that followed a volume fraction of 40 ： 50 ： 10; Column temperature was 30℃ ; Flow rate was 0.2mL/min. [ Results ] The retention time of melamine was 3.95 min. Melamine was linear in a range of 5-200μg/L with a coefficient square （R2） value of 0.999 8. At the concentration of 10, 50, and 100 μg/L, the recoveries ranged from 96.7% to 97.2% with relative standard deviations ≤ 5.16%. The limit of detection and limit of quantification were 0.6 μg/L and 2 μg/L, respectively. [ Conclusion ] The method is featured by simple pretreatment and high sensitivity, which is suitable for detecting melamine in human urine.