论文部分内容阅读
建立尿中氰离子的衍生化气相色谱-质谱联用测定方法。通过苯胺与亚硝酸盐生成的重氮盐与氰离子发生反应,衍生物用GC/MS/MS进行检测。优化了衍生化温度和时间、催化剂用量、衍生化试剂的用量等衍生化条件。在最佳条件下,氰离子衍生物稳定且色谱峰形良好,在0.1~10μg/m L范围内,检出限为0.030μg/m L,测量限为0.10μg/m L,相对标准偏差为4.61%,相对回收率为96.12%。该方法回收率高,专属性好,可用于尿中氰离子的定量测定。
Determination of cyanide ion in urine by gas chromatography - mass spectrometry method. The diazonium salts formed by aniline and nitrite reacted with cyanide ions and the derivatives were detected by GC / MS / MS. Derivatization conditions such as derivatization temperature and time, amount of catalyst and amount of derivatizing reagent were optimized. Under the best conditions, the cyanide derivatives were stable and the peak shape was good. The detection limit was 0.030μg / mL in the range of 0.1 ~ 10μg / mL, the limit of measurement was 0.10μg / mL, the relative standard deviation was 4.61%, the relative recovery rate was 96.12%. The method has high recovery rate and good specificity, and can be used for quantitative determination of cyanide ion in urine.