Determination Of Aminoglycoside Antibiotics Research Articles

Determination of aminoglycoside antibiotics in animal feed by high performance liquid chromatography using evaporative light scattering detector

This study was carried out to develop a method for the simultaneous analysis of 5-aminoglycosides such as streptomycin (STR), neomycin (NEO), kanamycin (KAN), spectinomycin (SPE), and amikacin (AMI) in animal feedstuffs using the (HPLC-ELSD) high performance liquid chromatography with Evaporative Light Scattering Detector detection. The 5-aminoglycoside antibiotics in animal feed samples were extracted with a solvent containing 20% ACN, 1% HCl (v/v). The extract was purified by solid-phase extraction (SPE) with the stationary phase of PCX, at pH 5 which was adjusted by NH3 solution. The 5-aminoglycosides were eluted from the SPR column with 10% NH3 solution. The eluted sample was evaporated to dryness and the residue was dissolved in 20 mM hepta fluorobutyric acid (HFBA) solution followed by filtering through a 0.22 µm membrane prior to analyze by HPLC – ELSD. The 5-aminoglycosides were separated on an Eclipse Plus C18, 1.8 µm, 4.6×100 mm column, an aqueous/acetonitrile containing 15 mM HFBA in gradient mode with ratio of H2O/ACN: 0-1 min fix at 76:25, 1-6 min reduce 55:45, 6-7 min fix at 55-45, 7-8 min increase to 75:25. A carrier gas velocity of the ELSD detector was 1 L/min and the misting temperature was 40oC. This method achieved a detection limit (MDL) of 4 mg/kg and a recovery yield of 87-92% for 5-aminoglycosides in feed sample with the HPLC – ELSD system.

ATR-FTIR Spectroscopy Methods for Determination of Aminoglycoside Antibiotics in Ophthalmic and Parenteral Preparations with Full Partial Least Squares Algorithm

ATR-FTIR Spectroscopy Methods for Determination of Aminoglycoside Antibiotics in Ophthalmic and Parenteral Preparations with Full Partial Least Squares Algorithm

Determination of amikacin by Rayleigh scattering method based on the covalent bonding of the analyte with a water soluble polymer

A method for the determination of aminoglycoside antibiotics based on the covalent bonding of the analyte with a water-soluble polymer by the Rayleigh scattering method (λex = λem) is proposed. Determination of amikacin (as a model analyte) is carried out by the carbodiimide crosslinking technique, which forms amide bonds between the copolymer of 4-styrenesulfonic acid and maleic acid and the primary amine groups of amikacin. The conditions of the reaction are selected to obtain maximum scattering intensity of the product: reaction time 15 min, pH 7.0, ionic strength 0.02, and measuring of scattering intensity at 362 nm. The determination of amikacin is not influenced by the following (mol/mol ratios): Al(III), Co(II), Cu(II), Fe(III), Ni(II), Zn(II)—300; Cl– and NO3-—250; Ca(II) and Mg(II)—50; HCO3-—20; it is affected by nitrogen compounds at 20–50-fold ratios and proteins at a 2.5-fold ratio. The calibration plot is constructed over the range of 0.2–35 mg/L (r = 0.993); LOD (3s-criterium) is 0.08 mg/L (n = 10, P = 0.95). Analyses are performed on drug powder for injection and gel.

A polyvinyl alcohol-functionalized sorbent for extraction and determination of aminoglycoside antibiotics in honey

A novel highly hydrophilic sorbent simply prepared by coating polyvinyl alcohol (PVA) onto silica gel was used for extraction and determination of aminoglycoside antibiotics (AAs). The fabricated PVA coating is aimed to effectively protect core silica gel inside and offers good hydrophilic property. In combination of hydrophilic interaction chromatography tandem mass spectrometry, the performance of the sorbent was evaluated by selecting four model AAs (dihydrostreptomycin, streptomycin, kanamycin, spectinomycin). The sorbent was found to have effective adsorption ability to hydrophilic AAs, which was superior or comparable to those of commercial ones. Good recoveries (84–112%) of model AAs spiked in honey were obtained with good precision (<12.4%) and the limit of quantitation for the proposed method was in the range of 7.8–19.4ng/mL.

Determination of Streptomycin and Dihydrostreptomycin in Honey by Liquid Chromatography–Electrospray Mass Spectrometry

A simple and reliable method using liquid chromatography–electrospray ionization‐mass spectrometry (LC/ESI‐MS) has been developed for the determination of aminoglycoside antibiotics, streptomycin (SM), and dihydrostreptomycin (DSM) in honey. The LC separation was performed on a TSK‐gel Super ODS column (100 × 2 mm i.d.) using 5 mM heptafluoro‐n‐butyric acid (HFBA)–acetonitrile (88:12) as the mobile phase at a flow rate of 0.18 mL/min. The positive ionization produced the typical (M + H)+ molecular ions of both drugs (SM m/z 582.3; DSM m/z 584.3). The calibration graphs for SM and DSM were rectilinear from 0.05 to 10 ng with selected ion monitoring (SIM). The drugs were extracted with water, and the extracts were cleaned up on an Oasis HLB cartridge (60 mg). The recoveries of both drugs from honey fortified at a level of 0.1 µg/g was 85.8–89.1%, with high precision. The limits of quantification of the drugs in honey were 0.01 µg/g (signal‐to‐noise ratio >10).

Resonance Rayleigh Scattering Method for the Determination of Aminoglycoside Antibiotics with Trypan Blue

In weak acidic medium, some aminoglycoside antibiotics, such as kanamycin (KANA), gentamicin (GEN), tobramycin (TOB), and neomycin (NEO), or acid bisazo dye trypan blue (TB) can only produce very weak resonance Rayleigh scattering (RRS) signals. However, when the two agents react with each other to form the ion association complexes, the RRS intensity can be enhanced greatly and a new RRS spectrum and a significant enhancement of the RRS intensity in the wavelength range 350–600 nm can be observed. The maximum scattering peak was at 580 nm. There is a linear relationship between the RRS intensity and the antibiotic concentration in the range 0.01–6.0 µg mL−1 at 580 nm. This RRS method has therefore been developed for the determination of trace levels of aminoglycoside antibiotics. The detection limits (3σ) of the four antibiotics, whose order of sensitivity KANA>NEO>TOB> GEN, are 6.1–8.1 ng mL−1. This method has a good selectivity and has been successfully applied to the quick determination of antibiotics not only for injections and ear dips, but clinic serum samples as well. In addition, quantum chemistry-based analysis of the reaction mechanism, the factors influencing the RRS spectra, and the reasons for the enhancement of RRS are discussed.

Evaluation of copper‐based electrodes for the analysis of aminoglycoside antibiotics by CE‐EC

AbstractAminoglycoside antibiotics including gentamicin, bekanamycin, tobramycin, lincomycin, neomycin, kanamycin, and ribostamycin have been determined by CE‐EC with copper clectrodes. Both copper wall‐jet electrodes (WJEs) and copper on‐capillary electrodes (OCEs) were evaluated. The OCEs provided μM detection limits, superior stability and reproducibility (2–3% relative standard deviation in oxidation current), and a simple instrumental set‐up without the need for capillary/electrode alignment. The analytical capabilities of the Cu‐OCE were examined, following the optimization of CE conditions, for the seven aminoglycosides above; and the practical utility of this approach was demonstrated through the determination of aminoglycoside antibiotics in three pharmaceutical preparations.

Kinetic fluorimetric determination of aminoglycoside antibiotics by use of OPA and N-acetylcysteine as reagents

The use of N-acetylcysteine for the kinetic fluorimetric determination of aminoglycoside antibiotics by reaction with o-phthaldialdehyde (OPA) in a basic medium was studied. The results obtained show that this thiol is a satisfactory substitute for 2-mercaptoethanol as reagent for the formation of isoindole derivatives of compounds containing primary amines such as amikacin, kanamicin and tobramycin, while avoiding its unpleasant odour. Due to the fast formation of the fluorescent derivatives the stopped-flow mixing technique must be used in order to acquire analytical kinetic data. This allowed the development of a kinetic automatic method for the determination of amikacin applicable to routine analyses. The initial rate was measured within ca. 5 s and the calibration graph was linear over the range 0.05–30.0 μg mL−1. The method was satisfactorily applied to the determination of amikacin in two pharmaceutical preparations with a mean recovery of 98.7%.

Determination of aminoglycoside antibiotics in pharmaceuticals by capillary zone electrophoresis with indirect UV detection coupled with micellar electrokinetic capillary chromatography

Aminoglycoside antibiotics can be determined by capillary zone electrophoresis (CZE) with indirect UV detection in the anionic mode with a reversed electroosmotic flow (EOF) by addition of FC 135 to the background electrolyte. The effective mobilities of thirteen aminoglycoside antibiotics were determined as a function of pH. Applying CZE with indirect UV detection in the anionic mode and reversed EOF coupled with micellar electrokinetic capillary chromatography with the cationic surfactant cetyltrimethylammonium bromide, both neutral and charged antibiotics can be determined in combined pharmaceuticals. As an example, neomycin and hydrocortisone were determined in Otosporin eardorps.

Determination of aminoglycoside antibiotics by reversed-phase ion-pair high-performance liquid chromatography coupled with pulsed amperometry and ion spray mass spectrometry

This work constitutes a preliminary investigation of a high-performance liquid chromatographic (HPLC)-mass spectrometric (MS) method for confirming aminoglycoside residues in bovine tissues. A reversed-phase ion-pair HPLC method for the separation of four aminoglycosides was developed using volatile ion-pairing agents and optimized for detection with an ion spray HPLC-MS interface. The method is also compatible with a commercial pulsed amperometric detector that was used for HPLC method development and that may be useful for the screening and quantification phases of a regulatory method. Several column phases, eluent compositions, and pairing ions were evaluated for optimum HPLC-MS sensitivity. Detection limits are in the low nanogram range with the pulsed amperometric detector and with HPLC-MS in the selected ion monitoring mode. Results with bovine kidney, fortified to 20 ppm and extracted by matrix solid-phase dispersion, obtained using both detectors are presented.

Determination of aminoglycoside antibiotics in biological fluids: a review.

We describe current procedures for measuring aminoglycoside antibiotics. Although many of these techniques are suitable for clinical adaptation, selection of a method for use in a clinical laboratory will depend on the budget and availability of equipment and expertise.