利用毛细管胶束电动色谱在线高盐堆积技术研究NaNOz-H202-氯高铁原卟啉(hemin)-酪氨酸(tyro-sine)体系中3-硝基酪氨酸(3-NT)的测定,建立了一种新的测定生物样品中微量3-NT的方法。最佳分离条件为:含SDS(30mmol/L)的Na2B407,(36mmol/L)缓冲液(pH9.3),进样压力为3.4kPa,进样时间为30s,毛细管柱温度25℃,分离电压20kV,样品中NaCl100mmol/L。在此条件下,3-NT检出限为0.1μmoL/L(S/N=3);线性范围为0.78~50ixmol/L;线性相关系数为0.9953。保留时间日内与日间的RSD(n=5)分别为1.6%和2.8%,加标回收率为95.2%~103.1%;样品不同浓度添加水平的日内和日间的RSD(n=5)均小于3%。本方法简单、快速、灵敏度高,为直接分析生物样品中的微量3-NT提供了方法。
A novel method for the quantification of minor 3-nitrotyrosine (3-NT) in NaNO2-H202-hemin-tyro- sine system was established by micellar electrokinetic chromatography with on-column high-salt stacking. The optimum CE separation conditions were achieved by using 36 mmol/L of Na2B40v as the running buffer contai- ning 30 mmol/L of SDS at pH 9.3, injection time of 30 s at pressure of 3.4 kPa ; separation voltage of 20 kV at temperature of 25℃ ; sample matrix containing 100 mmol/L of NaC1. Under the optimal CE conditions, the linear relationship ranged from 0.78 to 50 ixmol/L ( r = 0. 9953 ), and the limit of detection (LOD) was 0.1 Ixmol/L (S/N = 3). The RSDs of migration time for inter- and intra-day were 1.6% and 2. 8% , respectively. The recoveries were 95.2% - 103.1% and the RSDs for inter- and intra-day were less than 3% at various spiked levels. In this study, useful method is provided for the directly analysis of minor 3-NT in biological samples. The method is simple, rapid and sensitive.