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目的建立快捷准确测定尿液中亚硝酸盐含量的气相色谱-质谱(GC-MS)联用方法。方法通过优化衍生化过程中温度、时间和p H值等反应参数,建立2,3-二氨基萘(2,3-DAN)衍生化-GC-MS联用方法;采用亚硝酸盐阳性(NIT+阳性)尿液进行方法验证。结果尿液中NO-2经2,3-DAN衍生化后,色谱图分离度好、灵敏度高、峰形尖锐;线性方程为y=0.2071x+0.006,相关系数R2=0.999;本方法测定尿中亚硝酸盐的检测限为0.001μg/m L,线性范围0.01~20μg/m L,日内精密度(n=4)为3.19%~4.06%,日间精密度(n=5)为3.92%~5.16%,回收率为90.31%~113.5%;与现有方法比较,GC-M S联用方法具有检测限低、回收率、精密度高以及耗时短等优点。结论成功建立尿液中亚硝酸盐含量的GC-MS联用检测方法,该方法适用于法医鉴定及预防医学研究领域生物样品中亚硝酸盐痕量检测。
Objective To establish a rapid and accurate method for the determination of nitrite in urine by gas chromatography-mass spectrometry (GC-MS) combination method. Methods The derivatization of 2,3-diaminonaphthalene (2,3-DAN) -GC-MS was established by optimizing the reaction parameters such as temperature, time and p H value during derivatization. Nitrite-positive (NIT + Positive) urine for method validation. Results After the derivatization of NO-2 in urine by 2, 3-DAN, the chromatograms showed good resolution, high sensitivity and sharp peak shape. The linear equation was y = 0.2071x + 0.006, the correlation coefficient R2 was 0.999. The detection limit of mid-nitrite was 0.001 μg / mL with a linear range of 0.01 ~ 20 μg / mL. The intra-day precision was 3.19% -4.06% and the intraday precision was 3.92% (n = 5) ~ 5.16% and the recoveries ranged from 90.31% to 113.5%. Compared with the existing methods, GC-MS method has the advantages of low detection limit, high recovery, high precision and short time-consuming. Conclusion The method for the simultaneous determination of nitrite in urine by GC-MS was successfully established. This method is suitable for the detection of nitrite in biological samples in forensic medicine and preventive medicine research.