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目的建立以液质联用仪/离子阱(HPLC-MS/Trap)测定人尿中游离1-羟基芘(1-OHP)和1-羟基芘葡萄糖(1-OHP-G)的快速检测方法。方法尿样经过固相微萃取(SPE)法处理,二甲基亚砜复溶、离心取上清液分析;优化仪器的各种参数,10min内完成整个分析过程;1-OHP在m/z217.0～199.0离子对的跃迁和1-OHP-G在m/z413.3～301.2离子对的跃迁灵敏度最高。结果本方法能最低检测到8.4μg/L的游离1-OHP和12.5μg/L的1-OHP-G;尿样中的游离1-OHP和1-OHP-G含量:焦化工人分别为0.23和3.15μmol/molCr,普通居民分别为0.05和0.38μmol/molCr,接触组与对照组之间差异有显著性(P<0.05)。结论本方法分析时间短,HPLC-MS/Traps分析目标物受干扰少、特异性高,可作为一种评价多环芳香烃内负荷接触程度的有效方法。
Objective To establish a rapid method for the determination of 1-OHP and 1-OHP-G in human urine by HPLC-MS / Trap. Methods The urine samples were analyzed by solid-phase microextraction (SPE), dimethylsulfoxide re-dissolved, centrifuged and the supernatant was analyzed. The parameters of the instrument were optimized and the whole analysis process was completed in 10 minutes. The concentration of 1-OHP in m / z 217 . The transition of .0 ~ 199.0 ion pairs and the transition of 1-OHP-G at m / z 413.3 ~ 301.2 were the highest. Results The method could detect 8.4μg / L of free 1-OHP and 12.5μg / L of 1-OHP-G. The content of free 1-OHP and 1-OHP-G in urine samples were 0.23 3.15μmol / molCr, respectively. The average inhabitants were 0.05 and 0.38μmol / molCr, there was a significant difference between the contact group and the control group (P <0.05). Conclusions This method is short in analysis time and it can be used as an effective method to evaluate the contact degree of polycyclic aromatic hydrocarbons (PAHs) under the condition of low interference and high specificity by HPLC-MS / Traps analysis.