离子液体-分散液液微萃取-高效液相色谱法测定尿样中3-羟基苯并[a]芘  

Determination of urinary 3-hydroxybenzo [a] pyrene using ionic liquids-based dispersive liquid-liquid microextraction followed by high performance liquid chromatography with fluorescence detection

作　　者：胡欢[1] 徐志强[2] 杨俊[1] 林作敏 高芸[1] 淦五二[1] 

机构地区：[1]中国科学技术大学化学系,合肥230026 [2]安徽中烟工业有限责任公司技术中心,合肥230088

出　　处：《分析试验室》2016年第5期596-600,共5页Chinese Journal of Analysis Laboratory

基　　金：安徽中烟工业有限责任公司项目(2015124)资助

摘　　要：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 novel method for the sensitive determination of trace urinary 3-hydroxybenzo[a]pyrene of smokers was established using ionic liquids based dispersive liquid-liquid microextraction（ IL-DLLME） followed by high performance liquid chromatography（ HPLC） with fluorescence detection（ FLD）. The urine samples were hydrolyzed by enzyme and then enriched by IL-DLLME using 1-octyl- 3-methylimidazolium hexafluorophosphate as extraction solvent. Finally,the sedimented phase was injected into HPLC for analysis. Good linearity was obtained over a concentration range of 1. 5 - 150 ng / L with correlation coefficients（ r-2） of 0. 996. The enrichment factor was 180. The limit of detection（ LOD,S / N = 3） and limit of quantification（ LOQ,S / N = 10）values were 0. 45 and 1. 5 ng / L,respectively. The recoveries at spiked concentration levels of 1. 8 - 5 ng / L were between 85. 6% - 94. 6% with relative standard deviations of 3. 4% - 5. 2%. The method is simple,timesaving,sensitive,environmentally-friendly,reproducible with high precision and good recoveries and is suitable for the determination of urinary 3-OHBa P of smokers.

关 键 词：离子液体 分散液液微萃取 高效液相色谱法 尿样 3-羟基苯并[a]芘 

分 类 号：X830.2[环境科学与工程—环境工程]