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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 establish a method for the determination of phenol in urine by automatic headspace solid-phase microextraction (HS / SPME) -chromatography. Methods: The urine sample was acidified with hydrochloric acid and saturated with sodium chloride. The mixture was stirred at 60 ° C for 10 min, extracted with polyacrylate extraction head (PA, 75 μm) for 10 min and then desorbed at 260 ° C for 2.5 min. Separation was performed with FFAP capillary column. FID Detector detection. Results: The method showed good linearity in the range of 0 mg / L to 8.0 mg / L of phenol with a correlation coefficient r greater than 0.999 and a recovery of 87.1% -101.3%. The detection limit was 0.02 mg / L, the relative standard deviation is less than 4.2%. Conclusion: The method of automatic headspace SPME for the determination of phenol in the urine without organic solvents and the combination of extraction, concentration, desorption, injection and other functions is rapid, accurate and sensitive.