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建立了离子液体-分散液液微萃取/高效液相色谱-荧光检测法测定吸烟人群尿样中3-羟基苯并[a]芘的分析方法。尿样经酶解、滤膜过滤后,采用1-辛基-3-甲基咪唑六氟磷酸盐([C_8M IM][PF_6])为萃取剂进行分散液液微萃取富集,移取沉积相进行液相色谱分析。含量在1.5~150 ng/L范围内具备良好的线性关系(r~2≥0.996),富集倍数约为180。检出限(LOD,S/N=3)和测定下限(LOQ,S/N=10)分别为0.45和1.5 ng/L。在1.8~5 ng/L加标水平下,回收率为85.6~94.6%,相对标准偏差(RSD)为3.4%~5.2%。方法适用于吸烟人群尿样中痕量3-羟基苯并[a]芘含量的测定。
A method for the determination of 3-hydroxybenzo [a] pyrene in urine of smokers using ionic liquid-dispersive liquid-liquid microextraction / high performance liquid chromatography-fluorescence detection was established. After digestion of urine and filtration through the membrane, the sample was concentrated by liquid-liquid microextraction with 1-octyl-3- methylimidazolium hexafluorophosphate ([C_8M IM] [PF_6]) as extractant, The phases were analyzed by liquid chromatography. There was a good linearity (r ~ 2≥0.996) in the range of 1.5-150 ng / L, and the enrichment factor was about 180. The limits of detection (LOD, S / N = 3) and the lower limit of determination (LOQ, S / N = 10) were 0.45 and 1.5 ng / L, respectively. Under the spiked level of 1.8-5 ng / L, the recoveries ranged from 85.6% to 94.6%, and the relative standard deviations (RSDs) ranged from 3.4% to 5.2%. The method is suitable for the determination of trace 3-hydroxybenzo [a] pyrene in urine of smokers.