【摘要】 目的建立甲酯衍生化液液萃取-气相色谱法测定尿液中三氯乙酸的方法。方法在浓H₂SO₄催化下,尿液中的三氯乙酸与甲醇发生酯化反应,酯化产物通过正己烷液液萃取,离心,吸取有机相经无水硫酸钠干燥后注入气相色谱仪,经HP-INNOWAX毛细管色谱柱（30 m×0.32 mm,0.15μm）分离,采用氢火焰离子化检测器（FID）检测,以保留时间定性,峰面积定量。结果三氯乙酸在5.0 mg/L⁵00.0 mg/L呈线性关系,相关系数为0.999 6,以3倍噪音值估算方法的检出限为1.2 mg/L。在浓度为10.0 mg/L⁴00.0 mg/L低、中、高3个添加水平下,样品的加标回收率为95.2%⁹8.8%;批内精密度为1.24%².69%（n=6）,批间精密度为1.52%².22%（n=6）。结论本法简单实用,重现性好,灵敏度高,可以满足尿样中三氯乙酸检测的要求。更多还原

【Abstract】 Objective To establish a method for the determination of trichloroacetic acid in urine by liquid-liquid extractiongas chromatography after methylation derivatization.Methods Trichloroacetic acid was esterified by methanol with H₂SO₄ as catalyst.After extracting with n-hexane,and centrifuging,dehydrating by anhydrous sodium sulfate,the esterification product was separated by HP-IONOWAX capillary column（30 m×0.32 mm,0.15 μm）,and then detected by hydrogen flame ionization detector,with retention time for qualitative analysis and peak area for quantification.Results The detection limit of trichloroacetic acid in urine was 1.2 mg/L（S/N=3）,and the standard curve was linear in the range of 5.0 mg/L-500.0 mg/L（r=0.999 6）.The average recovery of trichloroacetic acid was 95.2%-98.8%at three spiked levels in the range of10.0 mg/L-400.0 mg/L.The intra-day and inter-day precisions（RSD） for the analysis were1.24%-2.69%（n=6） and1.52%-2.22%（n=6）,respectively.Conclusion The method is proved to be simple,practical,reproducible and highly sensitive.It can satisfy the request for the determination of trichloroacetic acid in urine.更多还原