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目的建立尿中三氯乙酸(TCA)的顶空气相色谱-质谱联用测定方法。方法尿中TCA加热脱羧生成三氯甲烷,经三合一自动进样器顶空进样,气相色谱柱分离,质谱检测器检测。结果 TCA在0.061 1～305.436 8μmol/L范围内线性良好(相关系数>0.999),最低检出浓度为0.009 2μmol/L(V=3 ml),不同浓度的相对标准偏差为4.5%～8.7%,样品加标回收率为82.0%～98.3%。结论本法简便、灵敏、准确,可同时应用于正常人群、职业接触人群和中毒病人的尿TCA的检测。
Objective To establish a method for the determination of trichloroacetic acid (TCA) in urine by headspace gas chromatography-mass spectrometry. Methods The TCA in urine was heated to decarboxylation to produce chloroform. The sample was injected into the headspace of a three-in-one autosampler, separated by gas chromatography and detected by mass spectrometry. Results TCA showed good linearity (correlation coefficient> 0.999) in the range of 0.061 1 ~ 305.436 8μmol / L with the lowest detection limit of 0.009 2μmol / L (V = 3 ml). The relative standard deviations of different concentrations were 4.5% ~ 8.7% The recoveries of spiked samples ranged from 82.0% to 98.3%. Conclusion This method is simple, sensitive and accurate and can be applied to the detection of urinary TCA in normal people, occupationally exposed people and poisoned patients.