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目的建立了尿中4-硝基苯代谢物4-硝基苯胺、4-硝基苯酚同时测定的高效液相色谱串联质谱方法。方法将10 ml样品过ENVI-18固相萃取柱富集,采用C18反相色谱柱分离,用甲醇和乙酸铵溶液为流动相进行梯度洗脱,质谱采用电喷雾正离子或负离子电离,多反应监测模式检测。结果 4-硝基苯胺、4-硝基苯酚分别在质量浓度为0.50μg/L~100.0μg/L和0.050μg/L~10.0μg/L时,具有良好的线性关系,相关系数(r)≥0.999 4,方法的检出限为0.002μg/L~0.02μg/L,回收率为87.2%~99.6%,相对标准偏差为2.6%~4.8%。结论此方法前处理简便、灵敏度高,具有良好的回收率和精密度。适用于尿中4-硝基苯代谢物即4-硝基苯胺、4-硝基苯酚的同时测定。
OBJECTIVE To establish a method for simultaneous determination of 4-nitroaniline and 4-nitrophenol in urine by high performance liquid chromatography-tandem mass spectrometry. Methods 10 ml samples were enriched by ENVI-18 SPE column, separated on a C18 reversed-phase column and eluted with methanol and ammonium acetate as mobile phases. The mass spectra were analyzed by electrospray positive ion or negative ion ionization, Monitoring mode detection. Results The results showed that 4-nitroaniline and 4-nitrophenol had good linearity when the concentration ranged from 0.50μg / L to 100.0μg / L and from 0.050μg / L to 10.0μg / L, respectively. The correlation coefficient 0.999 4. The detection limits were 0.002 μg / L ~ 0.02 μg / L, the recoveries were 87.2% -99.6%, and the relative standard deviations were 2.6% -4.8%. Conclusion This method is simple pre-treatment, high sensitivity, with good recovery and precision. For urine 4-nitrobenzene metabolites that 4-nitroaniline, 4-nitrophenol simultaneous determination.