scholarly journals Micellar Electrokinetic Chromatographic Study of the Separation of an Aromatase Inhibitor and a Tryciclic Antidepressant in the Breast Cancer Treatment

2008 ◽  
Vol 3 ◽  
pp. ACI.S939 ◽  
Author(s):  
J. Rodríguez Flores ◽  
A.M. Contento Salcedo ◽  
L. Muñoz Fernández

Micellar electrokinetic chromatography (MEKC) was investigated for the simultaneous determination of letrozole, imipramine and their metabolites in human urine samples over a concentration range of therapeutic interest. Experimental parameters such as pH of the running electrolyte, sodium dodecylsulphate (SDS) concentration, borate concentration, voltage, etc were investigated. Under optimal conditions of 25 mM SDS, 15 mM borate buffer (pH 9.2), 15% 2-propanol, as background electrolyte; 28 kV and 40 °C, as voltage and cartridge temperature, respectively; resolution between the peaks was greater than 1.7. Before the determination, a solid phase extraction (SPE) procedure with a C18 cartridge was optimized. Good linearity, accuracy, precision, robustness and ruggedness were achieved and detection limits of 12.5 ng/mL for letrozole and its metabolite and 37.5 ng/mL, were obtained for imipramine and their metabolites. Real determinations of these analytes in two patient urines were carried out. Sensitivity achieved in this method is sufficient to perform kinetic studies in humans.

2018 ◽  
Vol 2018 ◽  
pp. 1-9
Author(s):  
Qian Wang ◽  
Rui Zhao ◽  
Yan Cui ◽  
Cuicui Liu ◽  
Liya Liang ◽  
...  

A simple and rapid capillary electrophoresis method with diode array detector was developed for determination of sarafloxacin and difloxacin in beef. In this study, the experimental parameters affecting the determination were systematically optimized, including wavelength, buffer system, pH and concentration, and separation temperature and voltage. Under the optimal conditions, sarafloxacin and difloxacin could be quantified within 4 min using H3BO3/Na2B4O7 buffer (35 mmol/L, pH 8.8) as background electrolyte, 25 kV as separation voltage, and 22°C as the column temperature. The linear range of the method was 1–20 μg/mL with LOD 0.8 μg/mL for sarafloxacin and 0.5–20 μg/mL with LOD 0.3 μg/mL for difloxacin. The RSDs for the peak area of 8 μg/mL sarafloxacin were 4.8% (intraday) and 7.8% (interday), respectively. The proposed method has been applied to determine the residue of sarafloxacin and difloxacin in beef samples with the satisfactory recovery.


2019 ◽  
Vol 9 (6) ◽  
pp. 1193 ◽  
Author(s):  
Chih-Ying Huang ◽  
Yu-Xian Wang ◽  
Xin-Zhi Wang ◽  
Cho-Chun Hu ◽  
Tai-Chia Chiu

A low-cost, simple, and fast method utilizing micellar electrokinetic chromatography for the simultaneous determination of seven biogenic amines and two amino acids was developed. A background electrolyte containing 5 mM phosphate buffer (pH 3.7) and 20 mM sodium dodecyl sulfate was used. The optimal separation of nine investigated analytes was achieved in 11 min, with limits of detection (S/N = 3) ranging from 0.11 to 0.61 µM. The linear ranges for all analytes were observed between 0.55 and 10.0 μM (R2 > 0.990). The developed approach was extended to the analysis of analytes in commercial wine and beer samples. The recoveries of the proposed method ranged from 98.8% to 115.6%.


2016 ◽  
Vol 71 (2) ◽  
pp. 288-299 ◽  
Author(s):  
Mohamed M. Hassanien ◽  
Wael I. Mortada ◽  
Ibrahim M. Kenawy ◽  
Heba El-Daly

Amino silica gel functionalized with 2-hydroxy-5 -(2-hydroxybenzylideneamino)benzoic acid was synthesized, characterized and used as adsorbent for the removal of Ga3+, In3+ and Tl3+ from aqueous solution prior to their determination by flame atomic absorption spectrometry. Experimental parameters that affect the separation process were investigated in both batch and column modes. The maximum adsorption capacities of the sorbent are 61.7 mg g−1, 81.3 mg g−1 and 133.0 mg g−1 for Ga3+, In3+ and Tl3+, respectively. The preconcentration factor is 200 and the limits of detection of Ga3+, In3+ and Tl3+ are 4.10 μg L−1, 1.55 μg L−1 and 1.21 μg L−1, respectively. Interference by Al3+ can be masked by the addition of F−; and that of Fe3+ by its reduction to Fe2+ using 10% ascorbic acid. The method was successfully applied for the determination of these ions in water, sediments and liquid crystal display samples.


2016 ◽  
Vol 99 (2) ◽  
pp. 534-538 ◽  
Author(s):  
Yunus Emre Unsal ◽  
Mustafa Tuzen ◽  
Mustafa Soylak

Abstract An SPE of Au (III) on a 2-aminobenzothiazole–coated Diaion SP 207-column system has been developed. The parameters, including pH of solution, amount of 2-aminobenzothiazole, eluent type, sample volume, and flow rates, were examined. The effects of alkali, alkali earth, and some metals were also studied. The recovery values at optimal conditions and detection limits for Au (III) were found as >95% and 3.8 μg L−1, respectively. The factor of preconcentration was 250. The RSD value was <5%. The capacity of adsorption for the resin was 10.4 mg g−1. The accuracy of the method was evaluated by the use of CDN-GS-3D gold-certified reference material. The proposed procedure for the determination of gold was applied to water, mine, soil, and anodic slime samples.


2010 ◽  
Vol 8 (2) ◽  
pp. 273-277 ◽  
Author(s):  
Kateřina Vítková ◽  
Markéta Pechová ◽  
Jan Petr ◽  
Joanna Znaleziona ◽  
Václav Ranc ◽  
...  

AbstractA method for the fast determination of yohimbine, a potent adrenoreceptor antagonist used for the treatment of sexual dysfunctions, is proposed in this article. MEKC under basic and acidic conditions (sodium borate, pH 9.5 and sodium phosphate, pH 2.5) with SDS was developed. The effect of the experimental parameters, e.g. pH, SDS concentration and injection time, on yohimbine migration was also studied. Both methods were validated in terms of linearity, limits of detection and quantification, accuracy, and precision using caffeine as an internal standard. The application for the determination of yohimbine in hand-made medicaments is also investigated in this study.


Author(s):  
Syaza Azhari ◽  
Rahmalan Ahamad ◽  
Farediah Ahmad

A highly sensitive, rapid, simple and selective stripping assay for the determination of trace copper(II) is proposed.  The selectivity and sensitivity of the electroanalytical process on a glassy carbon (GC) electrode were enhanced using the newly synthesized Schiff base N,N’-bis(2-hydroxy-4-methoxyacetophenone)ethylenediamine (BME). The methodology is based on the accumulation of copper(II)–BME complex onto the GC electrode, followed by electrochemical oxidation of the adsorbed species. The effect of experimental parameters such as pH, BME concentration, scan rate, accumulation time and accumulation potential on the sensitivity of copper(II) detection were investigated. Under the optimal conditions, BME has successfully enhanced the copper(II) detection using the GC electrode by nearly 95% with detection limit (LOD) of  2.6 ngL−1. The effects of interfering ions such as Cd(II), Zn(II), Fe(II), Cr(III) and Pb(II) were also investigated. The applicability of this technique was illustrated by the determination of copper(II) ion in tap water.________________________________________GRAPHICAL ABSTRACT 


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