分析化学2012，Vol.40Issue(3)：397-402,6.DOI:10.3724/SP.J.1096.2012.10102
固相萃取-液相色谱-串联质谱法同时测定尿液中9种多环芳烃代谢物
SimultaneousDetermination of Nine Phenolic Metabolites of Polycyclic Aromatic Hydrocarbons in Human Urine by Liquid Chromatography Tandem Mass Spectrometry
摘要
Abstract
A method was developed for the simultaneous determination of nine phenolic metabolites of polycyclic aromatic hydrocarbons (OH-PAHs) in human urine, I, e. 2-hydroxynaphthaiene, 1-hydroxynaphthalene, 2-hydroxyfluorene, 3-hydroxyphenanthrene, 1-hydroxypyrene, 3-hydroxychrysene, 6-hydroxychrysene, 1-hydroxybenz[a] anthracenj 9-hydroxybenzo [a] pyrene by solidphase extraction-liquid chromatography tandem mass spectrometry (LC-MS/MS). After adding the internal standard (13 C3-Hydroxyphenanthrene) 1 the urine samples were hydrolyzed by enzyme (pH 5. 0) at 37℃ for 4 h, then cleaned up and concentrated on C18 SPE column, and then the targeted compounds were analyzed by LC-MS/MS under negative ion mode using Waters symmetry C18 column as analyzed column. The mobile phase was CH3CN∶NH3 ·HZO (0. 2%) = 72 = 27 (volume ratio). The spray voltage was 4 KV. The capillary temperature was 300℃. The linear ranges were 0.90 - 100 μg/L. The correlation coefficients were 0. 9970- 0. 9990. The detection limits were 0.04 -0.90μg/L. The recoveries were 79. 0% -119. 8%. The relative standard deviations were 4. 3% -12. 5%(n = 6). The method has been used for the simultaneous determination of nine phenolic metabolites of polycyclic aromatic hydrocarbons (OH-PAHs) in human urine.关键词
液相色谱串联质谱/尿/多环芳烃代谢物Key words
Liquid chromatography tandem mass spectrometry/ Urine/ Phenolic metabolites of polycyclic aromatic hydrocarbons引用本文复制引用
丁昌明,金银龙,林少彬..固相萃取-液相色谱-串联质谱法同时测定尿液中9种多环芳烃代谢物[J].分析化学,2012,40(3):397-402,6.基金项目
本文系国家“十一五”科技支撑基金(No.2006BAI19B01)资助项目 （No.2006BAI19B01）
