液相色谱-串联质谱法测定人尿中三聚氰胺
Liquid Chromatography-Tandem Mass Spectrometry for Determination of Melamine in Urine
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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，10 μL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 mL/min。
结果 三聚氰胺的保留时间3.95 min，三聚氰胺在5～200 μg/L的浓度范围内呈线性关系，
R 2为0.999 8。浓度在10、50、100 μg/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0.6 μg/L，最低定量限为2 μg/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。
Abstract:Objective To establish a method for melamine determination in human urine by liquid chromatographytandem 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 10 μL sample injection. The chromatographic conditions were as follows:Chromatographic column was CAPCELL PAK CR (SCX:C18=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 0.2 mL/min.
Results The retention time of melamine was 3.95 min. Melamine was linear in a range of 5-200 μg/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.
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