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目的建立同时测定尿液中萘、菲和芘的单羟基代谢产物1-羟基萘、2-羟基萘、3-羟基菲和1-羟基芘等的液相色谱-质谱检测方法。方法尿液样品经酶水解后,利用液液萃取进行净化提取,吹氮定容后进液相色谱质谱仪进行分析,利用内标标准曲线法对目标化合物进行定量。结果利用内标法进行定量分析,提高了方法的重现性和精密度,4种目标化合物的回收率在89.7%～103.0%范围内,批内和批间精密度分别在1.0%～4.2%和1.8%～5.8%范围内;1-羟基萘、2-羟基萘和1-羟基芘的检出限为0.2μg/L,3-羟基菲的检出限为0.1μg/L。结论液相色谱-质谱法灵敏度高,重现性和回收率好,适用于正常人群和多环芳烃暴露人群尿中1-羟基萘、2-羟基萘、3-羟基菲和1-羟基芘等多环芳烃代谢产物的检测。
OBJECTIVE To establish a liquid chromatography-mass spectrometry (LC-MS) method for the simultaneous determination of 1-hydroxynaphthalene, 2-hydroxynaphthalene, 3-hydroxy-phenanthrene and 1-hydroxypyrene in urine by single hydroxyl metabolites of naphthalene, phenanthrene and pyrene. Methods Urine samples were enzymatically hydrolyzed and purified by liquid-liquid extraction. Nitrogen was denatured and then analyzed by liquid chromatography-mass spectrometry. The target compounds were quantified by internal standard curve method. Results The internal standard method was used for quantitative analysis to improve the reproducibility and precision of the method. The recoveries of the four target compounds ranged from 89.7% to 103.0%, and the intra- and inter-batch precision were 1.0% -4.2% And 1.8% -5.8% respectively. The detection limits of 1-hydroxynaphthalene, 2-hydroxynaphthalene and 1-hydroxypyrene were 0.2μg / L and the detection limits of 3-hydroxy-phenanthroline were 0.1μg / L. Conclusion Liquid chromatography-mass spectrometry has the advantages of high sensitivity, reproducibility and good recovery. It is suitable for the determination of urinary 1-hydroxynaphthalene, 2-hydroxynaphthalene, 3-hydroxy-phenanthrene and 1-hydroxy-pyrene in normal population and PAH exposure groups Detection of PAHs Metabolites.