高效液相色谱—质谱法测定泌尿系结石中的三聚氰胺

Determination of melamine by high-performance liquid chromatography-mass spectrometry in urinary calculi

目的建立应用高效液相色谱—质谱法(LC/MS)检测泌尿系结石中三聚氰胺含量的方法。方法应用高效液相色谱—质谱法对17例因怀疑食用三聚氰胺污染奶粉在婴幼儿形成的泌尿系结石以及4例既往保存的成人尿酸结石进行三聚氰胺含量分析。采用正离子模式的电喷雾质谱检测。三聚氰胺最低检出限为0.1 mg/kg。结果 4例已知成人尿酸结石标本中均未检测到三聚氰胺,17例疑似标本中应用液相色谱—质谱联用仪分析后共4例标本中检测出三聚氰胺,含量浓度分别为0.8、0.5、1.2和64 mg/kg。结论高效液相色谱—质谱法准确度高、稳定性好,可以有效检测泌尿系结石中三聚氰胺含量,为进一步治疗和随访提供了帮助,但含三聚氰胺奶粉对患儿的长期影响还需进一步随访研究。

Objective To establish a high-performance liquid chromatography-mass spectrometry（LC//MS）-based method for efficient determination of melamine in urinary calculi in children taking melamine-contaminated formula milk powder.Methods LC/MS was employed to determine the contents of melamine in urinary calculi surgically removed from 17 children with a history of taking melamine-contaminated milk powder and in 4 samples of uric acid stone from adults.The positive ionization mode of electro-spray ionization source was used,and the limit of melamine determination was 0.1 mg/kg.Results No melamine was detected in the 4 uric acid stone samples from adults.Melamine was detected in 4 samples of urinary calculi from the 17 children,with the concentration ranging from 0.8 to 64 mg/kg.Conclusion LC/MS is simple and effective for detecting melamine in urinary calculi,which is helpful to the treatment and follow-up.