In order to evaluate the exposure to PAHs in environmental tobacco smoke, the influences of solid phase extraction column, chromatographic column and mass spectrometry conditions on analytical results were investigated, a method with SPE-HPLC/MS/MS was established to determine the biomarkers of 1-OHNap, 2-OHNap, 1-OHPyr, 6-OHChr, 3-OHFlu, 1-OHPhe, 2-OHPhe, 3-OHPhe, 4-OHPhe, 9-OHPhe and 2-OHFlu in human urine. Using l-OHNap-d8, 3-OHPhe-d9 and l-OHPyr-d9 as internal standards, the samples were hydrolyzed by ?-glucosidase/aryl sulfatase, extracted by Bond Elut C18 cartridge, separated by Eclipse PAH column, determined by mass spectrometry under multi-reaction monitoring mode (MRM), the OH metabolites of PAHs (OHPAHs) in urine were detected. The results showed that the limits of quantification (LOQ) of OHPAHs varied from 6 to 130 pg/mL. The detectable concentration of OHPAHs showed good linear relationship with r from 0.9991 to 1.0000, and the recoveries ranged from 72.45% to 124.50%. The intra-day and inter-day precisions were in the range of 1.49% to 7.35% and 2.90% to 12.00%, respectively. This method is suitable for simultaneously determining the biomarkers of PAHs in human urine.%为评估烟气环境中人体对多环芳烃的暴露状态,考察了固相萃取柱、色谱柱和质谱条件对分析结果的影响,建立了测定尿液中1-羟基萘(1-OHNap)、2-羟基萘(2-OHNap)、1-羟基芘(1-OHPyr)、6-羟基(屈)(6-OHChr)、3-羟基芴(3-OHFlu)、1-羟基菲(1-OHPhe)、2-羟基菲(2-OHPhe)、3-羟基菲(3-OHPhe)、4-羟基菲( 4-OHPhe)、9-羟基菲(9-OHPhe)、2-羟基芴(2-OHFlu)等11种多环芳烃生物标志物的固相萃取-液相色谱-串联质谱方法( LC-MS/MS).以1-羟基芘-d9(1-OHPyr-d9)、3-羟基菲-d9(3-OHPhe-d9)和1-羟基萘-d8(1-OHNap-d8)为内标,通过β-葡糖苷酸/芳基硫酸酯酶酶解、Bond Elut C18小柱固相萃取、Agilent ZORBAX Eclipse PAH色谱柱分离和多反应监测模式(MRM)质谱检测了尿液中多环芳烃的羟基代谢物(OHPAHs).结果表明,OHPAHs的定量限为6～130 pg/mL,r为0.9991～1.0000,加标回收率为72.45％～124.50％,日内精密度为1.49％～7.35％,日间精密度为2.90％～12.00％.该方法适用于尿液中多环芳烃生物标志物的分析.
展开▼
