[采用高效液相色谱-串联质谱法分析尿液中多环芳烃的单羟基代谢物]
[Using HPLC-MS/MS method to analyze monohydroxy metabolites of PAHs in urine].
作者信息
Huang Chuanfeng, Yan Huifang, Pan Zufei, Dai Yufei, Niu Yong, Wang Yujiang, Zheng Yuxin
机构信息
National Institute for Occupational Health and Poison Control, Chinese Center for Disease Control and Prevention, Beijing 100050, China.
出版信息
Wei Sheng Yan Jiu. 2010 May;39(3):355-7, 360.
OBJECTIVE
To establish a HPLC-MS/MS method for the simultaneous determination of 4 monohydroxy metabolites of polycyclic aromatic hydrocarbons (PAHs) in urine, including 1-naphthol, 2-naphthol, 3-phenanthrol and 1-pyrenol).
METHODS
After being treated by enzymatic hydrolysis, urine samples were purified by liquid-liquid extraction, evaporated under nitrogen to constant volume and examined by HPLC-MS/MS. Target compounds were quantified by internal standard calibration curve.
RESULTS
The reproducibility and precision were improved by internal standard calibration. The recovery of four target compounds were in the range of 89.7%-103.0%. The precision of intra- and inter-batch was 1.0%-4.2% and 1.8%-5.8% respectively. The limits of quantification was 0.2 microg/L for 1-naphthol, 2-naphthol and 1-pyrenol and the limits of quantification was 0.1 microg/L for 3-phenanthrol.
CONCLUSION
The sensitivity, reproducibility and recovery of HPLC-MS/MS method were good for the analysis of 1-naphthol, 2-naphthol, 3-phenanthrol and 1-pyrenol in the urine of people on occupational and nonoccupational exposure to PAHs.
目的
建立一种高效液相色谱-串联质谱法（HPLC-MS/MS），用于同时测定尿液中4种多环芳烃（PAHs）的单羟基代谢物，即1-萘酚、2-萘酚、3-菲酚和1-芘酚。
方法
尿液样品经酶解处理后，通过液液萃取进行净化，氮气吹干至恒容，然后用HPLC-MS/MS进行检测。目标化合物采用内标校准曲线进行定量。
结果
内标校准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%之间。批内精密度为1.0%-4.2%，批间精密度为1.8%-5.8%。1-萘酚、2-萘酚和1-芘酚的定量限为0.2μg/L，3-菲酚的定量限为0.1μg/L。
结论
HPLC-MS/MS法在分析职业和非职业接触PAHs人群尿液中的1-萘酚、2-萘酚、3-菲酚和1-芘酚时，具有良好的灵敏度、重现性和回收率。
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