Chen Q, Hu K, Miura Y
Center of Analysis and Measurement, Fudan University, Shanghai 200433, China.
Se Pu. 1999 Sep;17(5):480-2.
An ion chromatographic method was used to separate the species of L-ascorbic acid, sulfite and thiosulfate in their mixtures. This method is based on the separation of each anion in their mixtures by using a separation column, and then on the fluorimetric measurement of cerium (III) formed by a postcolumn reaction of cerium (IV) with the species of L-ascorbic acid, sulfite and thiosulfate in the effluent. The optimal conditions for separating and determining the above three species have been established. By using a 3 mmol/L carbonate eluent, the species of L-ascorbic acid, sulfite and thiosulfate could be eluted at the proper retention times of 1.7, 2.6 and 5.0 min, respectively, and these three anions could be separated completely. The effects of the concentrations of cerium (IV) and sulfuric acid in the postcolumn reaction solution on the chromatographic peak-height were tested in order to obtain the optimal peak-height. It was found that the peak-height at first increases rapidly with an increase in the concentration of cerium (IV) and sulfuric acid respectively up to a certain concertation, then increases slowly. These critical concentrations of cerium (IV) and sulfuric acid also depend on the amount of the analyte injected. Meanwhile the baseline signals of the sepectra increase with an increase in the concentration of cerium (IV). Some concentrations above the critical concentration of sulfuric acid could be selected as the optimal concentration of sulfuric acid, but the concentration of cerium (IV) should be optimized by establishing a compromise between the higher peak-height and the lower baseline signal. The detection limit of this method was found to be 1 mumol/L for thiosulfate when an amount of 100 microL analyte was injected.
采用离子色谱法分离L-抗坏血酸、亚硫酸盐和硫代硫酸盐混合物中的各组分。该方法基于使用分离柱分离混合物中的每种阴离子,然后对流出物中铈(IV)与L-抗坏血酸、亚硫酸盐和硫代硫酸盐反应生成的铈(III)进行荧光测量。已确定了分离和测定上述三种组分的最佳条件。使用3 mmol/L的碳酸盐洗脱液时,L-抗坏血酸、亚硫酸盐和硫代硫酸盐分别在1.7、2.6和5.0 min的适当保留时间被洗脱,这三种阴离子可被完全分离。测试了柱后反应溶液中铈(IV)和硫酸浓度对色谱峰高的影响,以获得最佳峰高。发现峰高起初分别随着铈(IV)和硫酸浓度的增加而迅速增加,直至达到一定浓度,然后缓慢增加。铈(IV)和硫酸的这些临界浓度也取决于进样分析物的量。同时,光谱的基线信号随着铈(IV)浓度的增加而增加。硫酸临界浓度以上的某些浓度可被选为硫酸的最佳浓度,但铈(IV)的浓度应通过在较高峰高和较低基线信号之间达成折衷来优化。当进样100 μL分析物时,该方法对硫代硫酸盐的检测限为1 μmol/L。