Ishio Nobuhiro, Fukushi Keiichi, Michiba Kanako, Takeda Sahori, Wakida Shin-Ichi
Research Institute for Marine Cargo Transportation, Kobe University of Mercantile Marine, Kobe, Japan.
Anal Bioanal Chem. 2002 Nov;374(6):1165-9. doi: 10.1007/s00216-002-1583-5. Epub 2002 Oct 17.
We have examined transient isotachophoresis (ITP) conditions, e.g. the nature of the terminating ion, its concentration, and the injection procedure, to improve the limit of detection (LOD) for determination of nitrite and nitrate in seawater by capillary zone electrophoresis (CZE). Artificial seawater containing 3.0 mmol L(-1) cetyltrimethylammonium chloride (CTAC) was used as background electrolyte (BGE). After sample injection 600 mmol L(-1) acetate was separately injected into the capillary as the terminating ion for transient ITP. The LOD for nitrite and nitrate, obtained at a signal-to-noise ratio (S/N) of 3, were 15 and 7.0 microg L(-1) (as nitrogen), respectively. Relative standard deviations (RSD) of peak area for nitrite and nitrate were 7.3 and 0.8%, respectively, and the RSD of peak height were 5.7 and 1.2%, respectively, when the concentrations of nitrite and nitrate were 0.05 and 0.25 mg L(-1). The RSD of migration time for these ions was 0.2%. The proposed method was applied to the determination of nitrite and nitrate in seawater samples. The results for nitrite were nearly in agreement with those obtained by naphthylethylenediamine spectrophotometric analysis (SPA; correlation coefficient 0.9041).
我们研究了瞬态等速电泳(ITP)条件,例如终止离子的性质、其浓度以及进样程序,以提高通过毛细管区带电泳(CZE)测定海水中亚硝酸盐和硝酸盐的检测限(LOD)。含有3.0 mmol L⁻¹十六烷基三甲基氯化铵(CTAC)的人工海水用作背景电解质(BGE)。进样后,将600 mmol L⁻¹乙酸盐作为瞬态ITP的终止离子分别注入毛细管中。在信噪比(S/N)为3时获得的亚硝酸盐和硝酸盐的LOD分别为15和7.0 μg L⁻¹(以氮计)。当亚硝酸盐和硝酸盐的浓度分别为0.05和0.25 mg L⁻¹时,亚硝酸盐和硝酸盐峰面积的相对标准偏差(RSD)分别为7.3%和0.8%,峰高的RSD分别为5.7%和1.2%。这些离子迁移时间的RSD为0.2%。所提出的方法应用于海水样品中亚硝酸盐和硝酸盐的测定。亚硝酸盐的结果与通过萘乙二胺分光光度分析(SPA)获得的结果几乎一致(相关系数0.9041)。