离子色谱法检测全血中的亚硝酸盐及其代谢产物

Ion chromatography determination of nitrite and its oxidative product in whole blood

目的建立全血中亚硝酸盐的离子色谱分析方法。方法将0.5mL全血和1mL水混合,用乙腈沉淀血液中的蛋白质后依次过C18柱、Ag柱和Na柱,用于去除其中的有机物和氯离子后进行离子色谱检测,并对蛋白沉淀溶剂、前处理柱等最佳实验条件进行考察。结果采用本文方法对空白添加全血进行检测,在色谱图上亚硝酸根离子及其氧化产物硝酸根离子的保留时间分别为10.02min、19.21min。选择乙腈作为蛋白沉淀剂,C18柱去除有机物,Ag柱去除氯离子,Na柱去除银离子。全血中亚硝酸根离子的检出限为0.05μg/mL,亚硝酸根和硝酸根的总回收率为95.9%~117.3%。结论本文方法简便,回收率好,灵敏度高,适用于中毒者血液中亚硝酸盐的检测。

Objective To establish a method for determination of nitrite in whole blood by ion chromatography. Methods 0. 5mL whole blood was mixed with 1 mL water, and the protein was precipitated with acetonitrile. It was passed through C18 column to remove organics and double connected mini-column of silver resin and a silver absorbing material to remove a high concentration of chloride ion usually present in whole blood. The filtrate was analyzed with ion chromatography. Results The retention time of nitrite ion and their oxidation products of nitrate were 10. 02min,19.21min respectively. Choose acetonitrile as protein precipitating agent, using C18 column to remove organics, Ag column to remove chloride ion, Na column to remove silver ions. Detection limit of nitrate in whole blood was about 0.05 μg/mL. The total recoveries of nitrite and nitrate were between 95.9% - 117.3%. Conclusion The method had high sensitivity and selectivity, and was suitable for the analysis of nitrite.