测定尿中三氯乙酸的自动顶空气相色谱法

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(r0.999),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。

Determination of trichloroacetic acid in urine by headspace gas chromatography

[Objective]To establish the method for determination of trichloroacetic acid in urine by headspace gas chromatography.[Methods]The trichloroacetic acid in urine was decarboxylated and formed into chloroform which was injected by auto headspace sampler,the chloroform was determined by capillary gas chromatography,FID spectrometry,quantified by external standard.[Results] There was a good linearity at the concentration of trichloroacetic acid between 0.1-100 mg/L(r>0.999),The limit of detection was 0.02 mg/L(v=5 ml).The proposed method was applied for analysis of urine samples and obtained the satisfactory results and good reproducibility with recoveries of 98.6%-99.7%.And the RSD of standard solution was 0.8%-2.6%.[Conclusion]The method is simple,sensitive and accurate.It is applicable to the detection of urinary trichloroacetic acid of people with exposure to trichloroethylene.