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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 establish a capillary gas chromatography method for the simultaneous determination of urinary N-methylformamide (NMF) and N, N-dimethylformamide (DMF). Methods: The pretreatment method of urine sample was optimized by uniform experimental design method, separated by HP-FFAP capillary column and detected by flame ionization detector. The retention time was qualitative and the internal standard method was used for quantification. Results: The linear range of NMF and DMF was 0.01 ~ 8.00μg / μl (r≥0.999). The detection limits of NMF and DMF were 5.0 × 10-4μg and 4.0 × 10-4μg respectively. The NMF and DMF The standard recoveries were 94.6% -105.0% and 98.0% -108.8%, respectively. Urine samples can be stored in a refrigerator at 4 ℃ for at least 14 days. Conclusion: The method is accurate, sensitive and has low detection limit. It is suitable for the simultaneous determination of N-methylformamide and N, N-dimethylformamide in urine.