Goldman R K, Vlessis A A, Trunkey D D
Department of Surgery, Oregon Health Sciences University, Portland 97201-3098, USA.
Anal Biochem. 1998 May 15;259(1):98-103. doi: 10.1006/abio.1998.2651.
A high-pressure liquid chromatography (HPLC) assay for measuring picomole quantities of nitrosothiol in biological samples was developed. The assay utilizes the catalytic reduction of nitrosothiol by mercuric cation (Hg2+). Released nitrogen oxide reacts with sulfanilamide (SA) and N-(1-napthyl)ethylenediamine (NNED) to form a stable azo dye. The azo dye is then separated from N-(1-napthyl)ethylenediamine and quantified by reversed-phase HPLC. In addition to nitrosothiol, nitrite and atmospheric nitrogen oxides are sources of nitrogen oxide that react with the reagents, SA and NNED, to form the azo dye. Therefore, a reference sample, which includes the nitrosothiol sample and all reagents except Hg2+, is utilized for the subtraction of nitrite and atmospheric nitrogen oxides which "contaminate" the nitrosothiol sample and reagents. This method is a sensitive (approximately 3 pmol; approximately 10(-1) microM) and accurate means to measure nitrosothiol concentration in biologic samples.
开发了一种用于测量生物样品中皮摩尔量亚硝基硫醇的高压液相色谱(HPLC)测定法。该测定法利用汞离子(Hg2+)对亚硝基硫醇的催化还原作用。释放出的氮氧化物与磺胺(SA)和N-(1-萘基)乙二胺(NNED)反应形成稳定的偶氮染料。然后将偶氮染料与N-(1-萘基)乙二胺分离,并通过反相HPLC进行定量。除了亚硝基硫醇外,亚硝酸盐和大气中的氮氧化物也是与试剂SA和NNED反应形成偶氮染料的氮氧化物来源。因此,使用一个参考样品(包括亚硝基硫醇样品和除Hg2+之外的所有试剂)来减去“污染”亚硝基硫醇样品和试剂的亚硝酸盐和大气中的氮氧化物。该方法是一种灵敏(约3皮摩尔;约10^(-1)微摩尔)且准确的测量生物样品中亚硝基硫醇浓度的方法。