顶空固相微萃取-气相色谱法测定尿中苯酚

Determination of phenol in human urine by HS/SPME-GC/FID

目的:建立了用自动顶空固相微萃取(HS/SPME)-气相色谱法测定尿中苯酚的测定方法。方法:尿样经盐酸酸化和氯化钠饱和,60℃搅拌平衡10 min,聚丙烯酸酯萃取头(PA,75μm)萃取10 min后,260℃下解吸2.5 min,用FFAP毛细管色谱柱分离,FID检测器检测。结果:本法在苯酚浓度0 mg/L～8.0 mg/L范围内呈良好的线性关系,相关系数r大于0.999,回收率在87.1%～101.3%之间,方法的检出限为0.02 mg/L,相对标准偏差小于4.2%。结论:自动顶空SPME法测定尿中苯酚,无需有机溶剂,集萃取、浓缩、解吸、进样等功能于一体,方法快速、准确、灵敏。

Objective：To develope a method for the determination of phenol in urine samples by gas chromatography with headspace solid-phase microextraction（HS/SPME）.Methods： The samples were acidified with hydrochloric acid and saturated with NaCl to maintain an agitating equilibrium at 60℃ for 10 min,headspace absorbed for 10 min using a 75 μm polyacrylate coated fiber and desorbed at 260℃for 2.5 min,and detected by GC/FID.Results： The linear range of the method was 0 mg/L^8.0 mg/L with the correlation coefficients（r） above 0.999.The average recoveries were in the range of 87.1%~101.3%,with relative standard deviation less than 4.2%.The detection limit of the method was 0.02 mg/L.Conclusion： The method is solvent-free and highly efficient in enrichment,deabsorption and injection,which is simple,convenient and practical,suitable for detection of phenol in urine samples.