毛细管气相色谱法同时测定尿中N-甲基甲酰胺和N,N-二甲基甲酰胺

Simultaneous determination of N-methylformamide and N,N-dimethylformamide in urine by capillary gas chromatography

目的：建立尿中N-甲基甲酰胺（NMF）和N,N-二甲基甲酰胺（DMF）同时测定的毛细管气相色谱法。方法：采用均匀试验设计法优化尿样的前处理方法,HP-FFAP毛细管色谱柱分离,火焰离子化检测器检测,保留时间定性,内标法定量。结果：NMF、DMF浓度在0.01-8.00μg/μl范围内线性关系良好（r≥0.999）;NMF和DMF的检出限分别为5.0×10^-4μg和4.0×10^-4μg;NMF和DMF的加标回收率分别为94.6%-105.0%和98.0%-108.8%。尿样在4℃冰箱中至少可保存14 d。结论：该方法准确、灵敏,检出限低,适用于尿中N-甲基甲酰胺和N,N-二甲基甲酰胺的同时测定。

Objective： To develop the capillary gas chromatographic analytical method for simultaneous determination of N-methylformamide（NMF） and N,N-dimethylformamide（DMF） in urine.Methods：Optimization on the sample pretreatment technique with uniform design was investigated.The urine samples were analyzed by capillary gas chromatography-flame ionization detector（GC-FID）.Retention time was used for qualitative analysis and internal standard method for quantitative analysis.Results：Calibration of both NMF and DMF were linear in the range of 0.01～8.00 μg/μl（r≥0.999）.The detection limit was 5.0×10^-4 μg and 4.0×10^-4 μg for NMF and DMF,respectively.The rates of recovery were 94.6%105.0% for NMF and 98.0%108.8% for DMF.The urine samples could be reserved at 4℃ for at least 14 days.Conclusion：The developed method with good accuracy and precision achieves lower limit of detection.The assay is suitable to determine NMF and DMF in urine simultaneously.