Recent progress in analytical capillary isotachophoresis

This review brings a survey of studies on analytical ITP published since 2016 until the first quarter of 2018 and includes chapters about theory and principles, instrumentation and techniques, and analytical applications of ITP. It shows the position of analytical ITP among contemporary separation techniques, where particularly its unique concentrating capabilities keep the interest to include it into novel high‐sensitivity analytical procedures. The reviewed papers are considered according to their nature, techniques used, and instrumentation employed. The significance of electrolyte system composition is emphasized by providing explicit values where possible.     

Recent progress in analytical capillary isotachophoresis

Capillary ITP is currently used as one of the most important tools for preseparation and preconcentration of trace analytes in complex or diluted samples. This contribution is a continuation of a series of regularly published reviews on the topic and covers the last 2 years. It brings a survey of related literature organized into following sections: theory and methodology, instrumentation and techniques, and applications.     

Assay of acebutolol in pharmaceuticals by analytical capillary isotachophoresis

Acebutolol [N-{3-acetyl-4-[(2-hydroxy-3-(isopropylamino)propoxy]phenyl} butanamide] is a cardioselective beta-blocker with a potent anti-hypertensive and antiarrhythmic effect. The optimised operational system of electrolytes for the newly developed ITP separation of acebutolol consisted of 10mM potassium acetate +10mM acetic acid (pH 4.65) as the leading electrolyte and 10mM beta-alanine with pH approximately 4 (adjusted with acetic acid) as the terminating electrolyte. The driving and detection currents were 75 and 20 microA, respectively and the analysis took approximately 13 min. Under these conditions the effective mobility of acebutolol was determined as 20.7 x 10(-9) m2 V(-1) s(-1). The calibration dependence was rectilinear in the range 0.14-1.4 mg ml(-1) of acebutolol base (r = 0.9995); relative standard deviation (RSD) values were 1.1% and 1.2% (n = 6) when determining 0.42 and 0.98 mg ml(-1) of acebutolol in a pure standard solution. The method, with the limit of detection (LOD) of 0.04 mg ml(-1) and limit of quantification (LOQ) of 0.12 mg ml(-1), was applied to the assay of acebutolol in Sectral tablets, Acecor tablets, Apo-acebutol tablets (nominal content 400 mg of acebutolol per tablet) and Acebirex tablets (nominal content 200 mg of acebutolol per tablet) with RSD = 0.7-1.7% (n = 6). No interference from any excipients present in the tablets was observed. The recoveries ranged from 98.8% to 102.4% as found by the standard addition technique.     

Instrumentation for capillary isotachophoresis

Modular instrumentation for capillary isotachophoresis provides an easy way to assemble a desirable configuration of the separation unit with respect to detection limits, load capacity, time and economy of analysis. New developments in the field may thus be quickly accepted.     

Investigations on the interferon-induced 2'-5' oligoadenylate system using analytical capillary isotachophoresis

The activity of the interferon inducible enzyme 2'-5' oligoadenylate synthetase (2-5A synthetase, E.C. 2.7.7) which converts ATP into a series of 2'-5' oligoadenylates was measured using analytical capillary isotachophoresis. The turnover rate of ATP during the reaction was monitored by determination of its concentration at the beginning and the end of the 2-5A synthetase reaction. The enzyme was analysed in extracts of peripheral blood mononuclear cells either pretreated or not with interferon.     

Recent progress in capillary isotachophoresis

This article is a continuation of previous reviews and summarizes the progress of analytical capillary isotachophoresis in the years 1997-1999. Papers reviewed include theoretical and methodological aspects as well as analytical applications. Included are also papers using isotachophoresis and/or isotachophoretic principles as part of multidimensional separation schemes.     

Recent progress in capillary isotachophoresis

This article is a continuation of previous reviews and summarizes the progress of analytical capillary isotachophoresis since 2000. Papers reviewed include methodological and instrumental aspects as well as analytical applications. Included are also papers using isotachophoresis and/or isotachophoretic principles as part of multidimensional separation schemes.     

Determination of imazalil by on-line coupled capillary isotachophoresis with capillary zone electrophoresis

A simple, rapid and reproducible capillary isotachophoretic on-line coupled with capillary zone electrophoresis (CITP-CZE) method for the determination of IMz in food packaging extracts and its residues in apples is described. A good separation of the IMZ from other sample constituents was achieved within 15 minutes without any sample clean up. Method characteristics (linearity, accuracy, intra-assay and detection limit) were determined. Less amount of time involved, sufficient sensitivity and low running cost are the important attributes of CITP-CZE method.     

Fully automated capillary isotachophoresis of proteins

An apparatus for fully automated capillary isotachophoresis was constructed. A commercial apparatus (Shimadzu IP-2A) was modified in the electrolyte pumping system and the flow lines were simplified. An automatic sampler was used for sequential sampling. The equipment, pumps, the sampler, a high-voltage DC power supply, and a recorder, were controlled by a system controller which comprises a microcomputer and a BASIC program for time-control of the equipments. The apparatus was successfully used for the automated sequential analysis of human serum proteins. Forty serum samples were analyzed within 17 h without manual operation and for each sample the serum proteins were resolved into about twenty UV peaks or shoulders.     

On-column radiometric detector for capillary isotachophoresis

An on-column radiometric detector for capillary isotachophoresis is described. Design of the detector follows its intended use, i.e., mainly the detection of¹⁴C labelled ionogenic compounds separable by this electromigration method. A key part of the detector is a small volume (70 or 200 nl) cell with the sensing part made of plastic scintillator with counting efficiencies of 13–15%. An equation correlating the precision of radioactivity measurements with physical and geometrical characteristics of the cell and isotachophoretic conditions has been derived providing a guide in optimizing both the geometrical dimensions of the cell and the isotachophoretic working conditions. A minimum detectability calculated for¹⁴C radionuclide (21 Bq for a 3 mm thickness of the sensing part of the cell) was in a good agreement with the value determined experimentally (16 Bq). Other parameters evaluated experimentally include resolving power, short- and long-term reproducibilities of the response. It was also shown that optimized driving current during the detection enables to improve the precision of the radioactivity measurement.     

Determination of domoic acid by on-line coupled capillary isotachophoresis with capillary zone electrophoresis

An on-line coupled capillary isotachophoresis--capillary zone electrophoresis (cITP-CZE) method for the determination of domoic acid in shellfish and algae is described. The optimised cITP-CZE electrolyte system was 10 mM HCl + 20 mM beta-alanine (BALA) + 0.05% hydroxyethylcellulose (leading electrolyte), 5 mM caproic acid (terminating electrolyte) and 20 mM caproic acid + 20 mM BALA + 0.1% HPMC (background electrolyte). A clear separation of the domoic acid from the other components of methanolic sample extract was achieved within 25 min. Method characteristics, i.e., linearity (0-200 microg/l), accuracy (recovery 101+/-3%), intra-assay repeatability (2.4%) and detection limit (1.5 microg/l) were determined. Speed of analysis, low laboriousness, high sensitivity and low running cost are the typical attributes of the cITP-CZE method. Developed method was successfully applied to analysis of shellfish samples and food supplements containing algae extract.