高效液相色谱-质谱联用定性定量分析尿液中N,N-二甲基色胺

Qualitative and quantitative analysis of N,N-Dimethyltryptamine in urine by high performance liquid chromatography-mass spectrometry

目的建立准确可靠的尿液中N,N-二甲基色胺定性定量分析方法。方法采用KinetexⓒC18(100×2.1 mm,2.6μm)色谱柱,乙腈和0.1%的甲酸及20 mmol醋酸铵梯度洗脱,流速0.5 mL/min。质谱条件:选用电喷雾离子源,在正离子电离模式下,采用多反应监测(MRM)的质谱扫描方式,N,N-二甲基色胺离子对为:m/z 189.8→58.1和m/z 189.8→145.0。结果N,N-二甲基色胺线性范围0.5~500 ng/mL,线性相关系数0.9897,最低检测浓度(LOQ,S/N=3)为0.5 ng/ml,空白添加回收率93.1%~99.3%。结论本研究建立的LC-MS/MS分析方法准确、快速、有效,可用于尿液中N,N二甲基色胺定性定量分析。

Objective To establish an accurate and reliable method for the qualitative and quantitative analysis of N,N-Dimethyltryptamine in urine.Methods KinetexⓒC18 column(100×2.1 mm,2.6μm)was used,the mobile phase consisted of acetonitrile and 0.1%formic acid,and the flow rate was 0.5 mL/min.Mass spectrometry was performed in multiple reaction monitoring(MRM)mode,with m/z of 189.8→58.1 and m/z of 189.8→145.0.Results The linear range was 0.5 to 500 ng/mL and the correlation coefficient was 0.9897.The limit of quantification(LOQ,S/N=3)was 0.5 ng/mL and the recovery of appended contrast in blank sample ranged from 93.1%to 99.3%.Conclusion The analysis method by LC-MS/MS in this study is accurate fast and effective,can be used can be used for qualitative and quantitative analysis of N,N-Dimethyltryptamine in urine.