Large volume sample stacking of cationic tetracycline antibiotics toward 10 ppb level analysis by capillary electrophoresis with UV detection.

This paper aimed to build up a sensitive CE method for the analysis of tetracyclines (TCs) antibiotics (including tetracycline, chlorotetracycline, oxytetracycline, and doxycycline) with conventional UV detection. Here, the large volume sample stacking was applied to achieve in capillary preconcentration of the targets. To achieve large volume sample stacking, the essential step was a large volume of sample (around 83.3% of total capillary length from inlet to detection window) hydrodynamically loaded. Then, the reserved voltage was added in order to push the sample matrix out of the capillary. Due to different pH between sample solution (pH 4.6) and BGE (pH 11.0), the cationic TCs would turn into negatively charged while the sample matrix was removing from the capillary. Finally, the anionic TCs were stacked at the inlet for the subsequent separation. Although the loss of sample existed during their charge transformation, the LODs could be improved around 40 times than that obtained by normal hydrodynamic injection CE method. Here, the LODs were in the range of 8.1-14.5 µg/L, around 10 ppb that close to the level by electrochemiluminescence or laser-induced fluorescence detection of TCs by CE. The precision was characterized by RSDs of migration times and peak areas, which were in the range of 0.19-0.24% and 0.97-2.54%, respectively. The recoveries of the developed method were in the range of 95-112% by spiking TCs in the tap water. The proposed inline preconcentration CE method could be a simple, speed, and sensitive method for the quantitative analysis of TCs.

Determination of trace amounts of boron in steels by on-line reaction/concentration/separation using an anion-exchange column.

A method for the on-line absorptiometric determination of trace amounts of boron in steels was developed using an anion-exchange column presorbed with chromotropic acid. The on-line reaction and separation were achieved by controlling the pH in order to accelerate the complex formation in the column by 2.7 and to stabilize the complex at pH 8 for the selective elution of a 1:2 complex and its detection at 350 nm. The effects from the iron matrix in the sample were effectively removed by using EDTA as a masking agent; a low limit for boron detection (3σ) of 0.04 µg g(-1) was obtained.

Anion exchanger as a reaction/separation medium-absorptiometric determination of trace amounts of boron in waters by on-line complexation with chromotropic acid presorbed on the anion-exchange column.

A novel method of on-line absorptiometric determination for trace amounts of boron was developed based on the complexation with chromotropic acid presorbed on an anion-exchange column. On-line reaction and separation were achieved by controlling pH conditions in solutions to accelerate the 1:2 complex formation in the concentration process at pH 3 and to stabilize the complex in the separation process at pH 8. About 75% of the boron introduced into the stream was kinetically collected as the 1:2 complex on the column under the experimental conditions. The 1:2 complex was satisfactorily separated from excess reagent and matrix components by changing the concentration of NaClO4 in the eluent and its peak height on the chromatogram monitored at 350 nm was used for calibration. The sensitivity could be enhanced by increasing the sample amount introduced and the detection limits (3sigma) were 162 ng dm(-3) and 45 ng dm(-3) of boron, when 5.0 cm3 and 13.4 cm3 of the samples were used, respectively. The method has been successfully applied to the determination of boron in samples of river water, tap water and ion-exchanged water.