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目的:探讨利用气相色谱-质谱(GC/MS)建立一种准确可靠的尿样中的N,N-二甲基乙酰胺(DMAC)及其代谢产物N-甲基乙酰胺(NMAC)的测定方法。方法:尿样经乙酸乙酯萃取、浓缩后,用GC/MS全扫描模式(scan)进行定性分析,确定组分出峰时间和特征质量离子,DMAC选择15、44、87m/z,NMAC选择30、43、73m/z,进行选择离子扫描(SIM),作定量分析。结果:DMAC和NMAC的线性范围分别为0.1 mg/L~10.0 mg/L和0.5 mg/L~10.0 mg/L;相关系数分别为0.9993和0.9991;最低检出限分别为0.02 mg/L和0.10 mg/L;相对标准偏差分别为3.26%和7.22%;样品加标回收率分别为91%~99%和88%~102%。结论:方法准确性好、灵敏度高、干扰少,是检测尿样中DMAC和NMAC的较好方法。
Objective: To investigate the determination of N, N-dimethylacetamide (DMAC) and its metabolite N-methylacetamide (NMAC) in urine by gas chromatography-mass spectrometry (GC / MS) method. Methods: Urine samples were extracted with ethyl acetate and concentrated. Qualitative analysis was performed with a GC / MS scan to determine the peak time of the components and the characteristic mass ions. The DMAC selection was 15, 44, and 87 m / z. The NMAC selection 30,43,73 m / z, selective ion scan (SIM), for quantitative analysis. Results: The linear range of DMAC and NMAC were 0.1 mg / L ~ 10.0 mg / L and 0.5 mg / L ~ 10.0 mg / L respectively, the correlation coefficients were 0.9993 and 0.9991, respectively. The minimum detection limits were 0.02 mg / L and 0.10, respectively mg / L; the relative standard deviations were 3.26% and 7.22% respectively; the spiked recoveries were 91% -99% and 88% -102% respectively. Conclusion: The method has good accuracy, high sensitivity and less interference. It is a better method to detect DMAC and NMAC in urine samples.