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目的建立人尿液中4种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)代谢产物的液相色谱-质谱(LC-MS-MS)同时测定法。方法尿液经过酶解,固相萃取净化富集,旋转蒸发浓缩,采用LC-MS-MS法检测尿中1-羟基芘、2-羟基芴、6-羟基屈、3-羟基苯并芘的浓度。结果在0.1～10μg/L的线性范围内,1-羟基芘、2-羟基芴、3-羟基苯并芘、6-羟基屈所得的回归方程均呈较好的线性关系(r≥0.999);该方法的检出限分别为0.2、0.15、0.2、0.2μg/L,该方法的平均回收率为61.3%～100.7%,RSD为1.5%～9.7%。结论该方法灵敏度高,重现性和回收率好,特异性高,适用于人尿样中PAHs单羟基代谢物的快速、大批量检测。
Objective To establish a liquid chromatography-mass spectrometry (LC-MS-MS) simultaneous determination of 4 metabolites of human polycyclic aromatic hydrocarbons (PAHs) in human urine. Methods Urine was purified by enzymolysis and SPE, concentrated by rotary evaporation. LC-MS-MS was used to detect urinary 1-hydroxypyrene, 2-hydroxyfluorene, 6-hydroxyl flexure and 3-hydroxybenzopyrene concentration. Results The linear regression equation of 1 - hydroxypyrene, 2 - hydroxyfluorene, 3 - hydroxybenzopyrene and 6 - hydroxyl flexion showed a good linearity (r ≥ 0.999) in the linear range of 0.1-10 μg / L. The detection limits of this method were 0.2, 0.15, 0.2 and 0.2 μg / L respectively. The average recoveries of this method ranged from 61.3% to 100.7% with RSD from 1.5% to 9.7%. Conclusion The method has high sensitivity, good reproducibility, good recovery and high specificity. It is suitable for rapid and high-throughput detection of monohydroxy metabolites of PAHs in human urine samples.