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目的建立尿中三氯乙酸的自动顶空气相色谱测定方法。方法尿中的三氯乙酸加热脱羧生成三氯甲烷,经自动顶空进样器进样,解吸后进气相色谱分离,FID检测,外标法定量。结果三氯乙酸在0.1～100mg/L浓度范围内线性良好(r>0.999),最低检出浓度为0.02 mg/L(v=5 ml),方法准确度高,重现性好,样品加标回收率为98.6%～99.7%,相对标准偏差(RSD)为0.8%～2.6%。结论该法简便、灵敏、准确,适用于三氯乙烯接触人群尿三氯乙酸的检测。
Objective To establish a method for the determination of trichloroacetic acid in urine by automated headspace gas chromatography. Methods Trichloroacetic acid in urine was heated to decarboxylation to produce chloroform. The sample was taken by automatic headspace sampler and was separated by gas chromatography after desorption. FID was detected by external standard method. Results Trichloroacetic acid showed a good linearity (r> 0.999) in the range of 0.1-100 mg / L with the lowest detectable concentration of 0.02 mg / L (v = 5 ml). The method showed high accuracy and good reproducibility. The recoveries ranged from 98.6% to 99.7%, and the relative standard deviations (RSDs) ranged from 0.8% to 2.6%. Conclusion The method is simple, sensitive and accurate and is suitable for the detection of urinary trichloroacetic acid in trichlorethylene exposure groups.