目的建立人尿中三聚氰胺和三聚氰酸的亲水作用液相色谱-电喷雾串联质谱法,对门诊病人尿液中三聚氰胺和三聚氰酸进行调查。方法样品加入同位素内标后采用亲水性键合硅胶和阳离子交换树脂复合填料固相萃取小柱(MCT)浓缩净化,甲醇和5%氨水甲醇溶液两次洗脱,收集流出液,用氮气吹干,用1 ml乙腈+2 mmol/L乙酸铵(90+10)充分溶解后,亲水作用色谱柱分离,采用电喷雾串联四极杆质谱进行检测。结果在2.0μg/L~1000.0μg/L时,三聚氰胺和三聚氰酸线性关系良好(相关系数r分别为0.9998和0.9997)。在50.0 ng/L、200.0 ng/L和5000 ng/L 3个添加水平范围内的平均回收率为97.8%~100.1%,相对标准偏差小于4.02%,方法检出限为三聚氰胺4.0 ng/L、三聚氰酸3.0 ng/L。结论采用建立的方法测定了尿中三聚氰胺和三聚氰酸,结果表明,该法快速、准确、灵敏,优于现有分析方法。 Objective To establish a hydrophilic interaction of melamine and cyanuric acid in human urine by liquid chromatography-electrospray ionization tandem mass spectrometry to investigate melamine and cyanuric acid in urine of outpatients. Methods After adding isotope internal standard, the samples were concentrated and purified with hydrophilic bonded silica gel and cation exchange resin composite packed solid phase extraction cartridge (MCT). The methanol and 5% aqueous ammonia solution were eluted twice, and the effluent was collected and purged with nitrogen Dried, and fully dissolved with 1 ml of acetonitrile + 2 mmol / L ammonium acetate (90 + 10). The mixture was separated on a hydrophilic column and detected by electrospray tandem quadrupole mass spectrometry. The results showed good linearity between melamine and cyanuric acid at 2.0μg / L to 1000.0μg / L (r = 0.9998 and 0.9997, respectively). The average recovery within the range of 50.0 ng / L, 200.0 ng / L and 5000 ng / L was 97.8% -100.1% and the relative standard deviation was less than 4.02%. The detection limits were 4.0 ng / L for melamine, Cyanuric Acid 3.0 ng / L. Conclusions The urinary melamine and cyanuric acid were determined by the established method. The results showed that the method was rapid, accurate and sensitive, which was better than the existing methods.