Capillary Electrophoresis analysis of gentamicin sulphate with UV detection after pre-capillary derivatization with 1,2-phthalic dicarboxaldehyde and mercaptoacetic acid

Kaale, Eliangiringa; Leonard, Stefanie; Schepdael, Ann Van; Roets, Eugène; Hoogmartens, Jos

doi:10.1016/s0021-9673(00)00412-x

Cited by 59 publications

(40 citation statements)

References 34 publications

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“…The advantages of gentamicin over other aminoglycosides (kanamycin, neomycin) are its activity towards Pseudomonas aeruginosa and microorganisms of the Serratia-Klebsiella -Enterobacter group, a faster bactericidal effect, and the rare development of gentamicin resistant strains [1]. It can be quantified using colorimetric technique [2], amperometric enzyme-immunosensors [3], flow injection chemiluminescence [4], spectrofluorometry [5][6][7], capillary electrophoresis with UV detection [8], liquid chromatography (LC) [9][10][11][12][13][14] and high performance liquid chromatography (HPLC) [15][16][17][18][19][20][21][22][23].…”

Section: Introductionmentioning

confidence: 99%

Indirect spectrophotometric determination of gentamicin and vancomycin antibiotics based on their oxidation by potassium permanganate

et al. 2006

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Four simple, accurate, sensitive and economical procedures (A -D) for the estimation of gentamicin sulphate and vancomycin hydrochloride, both in pure form and in pharmaceutical formulations have been developed. The methods are based on the oxidation of the studied drugs by a known excess of potassium permanganate in sulphuric acid medium and subsequent determination of unreacted oxidant by reacting it with amaranth dye (method A), acid orange II (method B), indigocarmine (method C) and methylene blue (method D), in the same acid medium at a suitable λ max =521, 485, 610 and 664 nm, respectively. The reacted oxidant corresponds to the drug content. Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 4-8, 3-8, 4-9 and 5-9 µg ml −1 with gentamicin and 4-8, 1.5-4, 1.5-4 and 3.5-5.5 µg ml −1 with vancomycin for methods A, B, C, and D, respectively. The molar absorptivity, sandell sensitivity, detection and quantification limits were calculated. The stoichiometric ratios for the cited drugs were studied. The optimum reaction conditions and other analytical parameters were evaluated. The influence of the substance commonly employed as excipients with these drugs were studied. The proposed methods were applied to the determination of these drugs in pharmaceutical formulations. The results have demonstrated that the methods are equally accurate and reproducible as the official methods.

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Section: Introductionmentioning

confidence: 99%

Indirect spectrophotometric determination of gentamicin and vancomycin antibiotics based on their oxidation by potassium permanganate

et al. 2006

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“…Analysis of gentamicin by CE with UV detection after precapillary derivatization with phthalic dicarboxaldehyde (OPA)/mercaptoacetic acid (MAA) was reported by Kaale et al [21] with concentration limit of quantitation (LOQ) values of the four major gentamicin components ranging from 0.3 mg/L to 1.0 mg/L. Electrophoretically mediated microanalysis of gentamicin with in-capillary derivatization was also investigated by the same authors [22], with LOQ ranging from 1.0 mg/L to 2.5 mg/L.…”

Section: Introductionmentioning

confidence: 99%

Gentamicin assay in human serum by solid-phase extraction and capillary electrophoresis

Kaale¹,

Long

Fonge

et al. 2005

Electrophoresis

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We describe the development of a capillary electrophoresis method for the determination of gentamicin C1, C1a, C2a, and C2 components in human serum. Using a weak cation-exchanger with 20 mM phosphate buffer, pH 7.4, 200 mM borate buffer, pH 9.0, and ammonia/methanol, solid-phase extraction (SPE) of gentamicin components from the human sera was performed. The extract was derivatized with 1,2-phthalic dicarboxaldehyde/mercaptoacetic acid reagent. The derivatives were separated with a background electrolyte comprising 60 mM 2-(N-cyclohexylamino)ethanesulfonic acid (CHES) buffer at pH 9.5 containing 31.6% m/v methanol, and quantified with UV-light absorption detection at 230 nm. The identity of the gentamicin components was confirmed by mass spectrometry. The SPE recovery of the gentamicin ranged from 78% to 93%. The calibration curves were linear from the concentration limit of quantitation (LOQ) to 30 mg/L for the gentamicin mixture. The LOQ for gentamicin C1 was 0.33 mg/L, for C2a 0.23 mg/L, C2 0.25 mg/L, C1a 0.27 mg/L and the concentration limit of detection (LOD) for C1 was 0.15 mg/L, C2a 0.11 mg/L, C2 0.12 mg/L, C1a 0.13 mg/L. Intra-assay relative standard deviation (RSD) values were for C1 (5%), C1a (7%), C2 (6.5%) and C2a (9%); inter-assay RSD values were for C1 (11%), C1a (13.3%), C2 (15%) and C2a (14%). The Pearson's correlation between capillary electrophoresis and immunoassay revealed a linear relationship between these two techniques with r = 0.9. This method for determination of gentamicin C1, C1a, C2a, and C2 in human serum can thus be used in the entire therapeutic concentrations range of gentamicin.

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“…Normally derivatization is required to detect gentamicin because of its lack of UV chromatophore [13][14][15][16][17]. Postcolumn or precolumn derivatizations by 1,2-phthalic dicarboxaldehyde (OPA), dansylchloride and mercaptoacetic acid (MAA) with either UV or fluorescence detection have been reported [13][14][15][16][17]. Although these detection methods are quite sensitive, the derivatization step is time-consuming and needs well-controlled experimental conditions to get reproducible results.…”

Section: Introductionmentioning

confidence: 99%

Direct determination of gentamicin components by capillary electrophoresis with potential gradient detection

Yuan

Wei

2005

Electrophoresis

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A simple and fast method was developed to determine non-UV active compounds directly without derivatization. The usefulness of the method was demonstrated by detecting the major components in aminoglycoside antibiotic mixtures using capillary zone electrophoresis with potential gradient detection. Under optimized separation conditions (0.2 mM cetyltrimethylammonium bromide (CTAB), 1 mM ammonium citrate, pH 3.5), gentamicin was separated into three major peaks (C1, C1a, and C2+C2a) within 15 min. This method showed better sensitivity than other capillary electrophoresis (CE) methods for determining underivatized gentamicin. The linear range was from 10 to 500 ppm. Because of its good repeatability and simplicity, this new method could be a good alternative for the current assays given by US Pharmacopoeia and European Pharmacopoeia.

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Capillary Electrophoresis analysis of gentamicin sulphate with UV detection after pre-capillary derivatization with 1,2-phthalic dicarboxaldehyde and mercaptoacetic acid

Cited by 59 publications

References 34 publications

Indirect spectrophotometric determination of gentamicin and vancomycin antibiotics based on their oxidation by potassium permanganate

Indirect spectrophotometric determination of gentamicin and vancomycin antibiotics based on their oxidation by potassium permanganate

Gentamicin assay in human serum by solid-phase extraction and capillary electrophoresis

Direct determination of gentamicin components by capillary electrophoresis with potential gradient detection

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