Determination of azide in gastric fluid and urine by flow-injection electrospray ionization tandem mass spectrometry
Determination of azide in gastric fluid and urine by flow-injection electrospray ionization tandem mass spectrometry
复制标题
流动注射电喷雾电离串联质谱法测定胃液和尿液中的叠氮化物
DOI：
10.1007/s00216-012-5848-3
复制
发表时间：
2012
期刊：
影响因子：
--
通讯作者：
Hideki Nozawa
中科院分区：
文献类型：
--
作者：
Kayoko Minakata;Hideki Nozawa
建立了一种快速测定胃液和尿液中叠氮离子（N3-）的方法。稀释后的生物体液中的N3-与NaAuCl 4反应生成Au（N3）2-，用正辛醇萃取。将五微升提取物流动注射到电喷雾电离串联质谱仪中。在10 min内使用50 μL水溶液，通过产物离子Au（N）（N3）-atm/z253的选择反应监测进行N3-的定量，产物离子源自前体离子Au（N3）2-atm/z281。方法的线性范围为10 ~（-5）M，定量限为10 ~（-7）M，检出限为3.0 × 10 ~（-8）M，变异系数为10%~ 10%。对于尿液，向50 μL尿液中加标N3-，将其稀释10倍并通过1 mL树脂，最后稀释至原始浓度的100倍。方法的线性范围为10 ~（-3）M，定量限为10 ~（-5）M，检测限为3.0 × 10 ~（-6）M，对10 ~（-5）M的尿样进行检测，变异系数为8.8%。通过将1 μL疑似自杀受害者的胃液稀释20，000倍和将1 μL受害者的尿液稀释5，000倍，然后测量N3-水平，来检查该方法的实用性。这些水平分别为（7.5 ± 1.0）× 10- 2 M和（3.2 ± 0.4）× 10- 3 M。图对于叠氮化物，观察到的产物离子为atm/z 253、225和42，而对于OCN，仅观察到atm/z 42。
A rapid method was developed to identify and quantify the azide ion (N3–) in gastric fluid and urine. N3–in diluted biological fluids was reacted with NaAuCl4to produce Au(N3)2–, which was extracted with octanol. Five microliters of the extract were flow-injected into an electrospray ionization tandem mass spectrometric instrument. Quantification of N3–was performed by selected reaction monitoring of the product ion Au(N)(N3)–atm/z253, which was derived from the precursor ion Au(N3)2–atm/z281, using 50 μL of aqueous solution within 10 min. This method was found to be linear up to 10–5M, to have a limit of quantification of 10–7M, a limit of detection of 3.0 × 10–8M, and a coefficient of variation of ≦10% at 10–7M. In the case of urine, 50 μL of urine were spiked with N3–, this was diluted 10-fold and passed through 1 mL of a resin, and finally diluted to 100-fold of the original. This method was linear up to 10–3M, had a limit of quantification of 10–5M, a limit of detection of 3.0 × 10–6M, and coefficient of variation of ≦8.8% for an original urine concentration of 10–5M. The practical applicability of this method was checked by diluting 1 μL of a suspected suicide victim’s gastric fluid 20,000-fold and 1 μL of the victim’s urine 5,000-fold and then measuring the N3–levels. These levels were found to be (7.5 ± 1.0) × 10–2M and (3.2 ± 0.4) × 10–3M, respectively.FigureThe product ions were observed atm/z253, 225 and 42 for azide but that was observed only atm/z42 for OCN.