尿液中亚硝酸盐2,3-二氨基萘衍生化-GC-MS联用法测定

Determination of nitrite in urine by 2,3-diaminonaphthalene derivatization-GC-MS

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 develop a rapid and accurate gas chromatography-mass spectrometry（ GC-M S） method for the determination of nitrite in urine. Methods Through optimizing operation parameters as temperature,time,and p H of derivatization,we developed a 2,3-diaminonaphthalene derivatization-GC-M S method for the determination of nitrite in urine. Results This method was sensitive,reproducible and accurate. The equation for the regression line was y =0. 207 1x ＋ 0. 006（ R2= 0. 999）; the linear range was 0. 01- 20 μg / m L; the limit of detection（ LOD） was 0. 001 μg / m L;the intra-day relative standard deviation（ % RSD） was 3. 19- 4. 06% and the inter-day % RSD was 3. 92- 5. 16%; the recovery was 90. 31%- 113. 5%. Conclusion The method has lower detection limit,better recovery,higher precision,and less time-consuming performance and could be applied in forensic and preventive medicine analysis.