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Ion selective electrodes for stability-indicating determination of gemifloxacin mesylate
Abstract
Three novel polyvinyl chloride (PVC) membrane sensors for the determination of gemifoxacin mesylate are described and characterized. The sensors are based on the use of the ion association complexes of gemifoxacin cation with ammonium reineckate counter anions as ion exchange sites in the PVC matrix. The membranes incorporate ion association complexes of gemifoxacin with dibutylsebathete (sensor 1), dioctylphthalate (sensor 2), nitrophenyl octyl ether (sensor 3). The performance characteristics of these sensors were evaluated according to IUPAC recommendations, which reveal a fast, stable and linear response for gemifoxacin over the concentration range of 10-5-10-2 M for the three sensors with cationic slopes of -14.30, -20.44 and -22.37 mV per concentration decade for the three sensors, respectively. The proposed sensors displayed useful analytical characteristics for the determination of gemifoxacin mesylate in bulk powder, pharmaceutical formulation, and biological fluids (plasma) and in the presence of its acid degradation products and thus could be used for stability-indicating studies. Validation of the method shows suitability of the proposed sensors for use in the quality control assessment of gemifoxacin mesylate. The developed method was found to be simple, accurate and precise when compared with a manufacturer HPLC method.
... Molecules 2023, 28, 5144 2 of 14 [29]. The published potentiometric methods [26][27][28] for GF measurement were based on the utilization of coated wire [26], ZnO nanorod [27], and ion-pair as electroactive materials in PVC matrix [28]. Ionophores were used as the sensing materials in the current investigation, which focused on host-guest interaction. ...
... According to a literature review, analytical methods used for the determination of gemifloxacin include spectrophotometry [6][7][8], spectrofluorometry [9,10], polarography [11], voltammetry [12][13][14], HP-TLC [15,16], HPLC-UV [17][18][19] , HPLC-F [20][21][22], HPLC-MS [23][24][25], and potentiometry [26][27][28][29]. Numerous studies have focused on the use of potentiometric ion-selective electrodes to assess distinct active ingredient drugs that employ various cyclodextrins (CD) and calixarene modifiers based on the host-guest inclusion process [30,31]. ...
... Potentiometric techniques based on membrane sensors are simple, affordable, precise, quick to respond, and unaffected by the presence of samples with color or turbidity [29]. The published potentiometric methods [26][27][28] for GF measurement were based on the utilization of coated wire [26], ZnO nanorod [27], and ion-pair as electroactive materials in PVC matrix [28]. Ionophores were used as the sensing materials in the current investigation, which focused on host-guest interaction. ...
Supramolecular gemifloxacin (GF) sensors have been developed. Supramolecular chemistry is primarily concerned with noncovalent intermolecular and intramolecular interactions, which are far weaker than covalent connections, but they can be exploited to develop sensors with remarkable affinity for a target analyte. In order to determine the dose form of the quinolone antibacterial drug gemifloxacin, the current study's goal is to adapt three polyvinylchloride (PVC) membrane sensors into an electrochemical technique. Three new potentiometric membrane sensors with cylindric form and responsive to gemifloxacin (GF) were developed. The sensors' setup is based on the usage of o-nitrophenyl octyl ether (o-NPOE) as a plasticizer in a PVC matrix, β-cyclodextrin (β-CD) (sensor 1), γ-cyclodextrin (γ-CD) (sensor 2), and 4-tert-butylcalix[8]arene (calixarene) (sensor 3) as an ionophore, potassium tetrakis (4-chlorophenyl) borate (KTpClPB) as an ion additive for determination of GF. The developed method was verified according to IUPAC guidelines. The sensors under examination have good selectivity for GF, according to their selectivity coefficients. The constructed sensors demonstrated a significant response towards to GF over a concentration range of 2.4 × 10-6, 2.7 × 10-6, and 2.42 × 10-6 mol L-1 for sensors 1, 2, and 3, respectively. The sensors showed near-Nernstian cationic response for GF at 55 mV, 56 mV, and 60 mV per decade for sensors 1, 2, and 3, respectively. Good recovery and relative standard deviations during the day and between days are displayed by the sensors. They demonstrated good stability, quick response times, long lives, rapid recovery, and precision while also exhibiting good selectivity for GF in various matrices. To determine GF in bulk and dose form, the developed sensors have been successfully deployed. The sensors were also employed as end-point indicators for titrating GF with sodium tetraphenyl borate.
... Potentiometric methods, using ion selective electrodes, have found wide application [16,17] being simple analysis procedures, economical coasts, fast results , applicable over a wide range of concentrations, applicability to various drug forms, with applicability to turbid and colored solutions, preciseness and offering enough selectivity towards the drug in the presence of various pharmaceutical excipients. ...
... The membranes incorporate ion association complexes of GEMI with dibutylsebathete, dioctylphthalate, nitrophenyl octyl ether. The proposed sensors were successfully applied for determination of GEMI in bulk powder, pharmaceutical formulation, and biological fluids [17]. ...
... The testing series was prepared by adding adequate amount of (0.2 electrode potential was observed in pH range from 2 to 3 and decreased from pH 4 to 11, Figure 4. These result suggested that the inclusion complex of GEMI and HPβ-CD was suitable in acidic media because GEMI containing primary amine group that capable to bind with protons presents in acidic media resulting positively charged GEMI ion, which therefore can attracted by anionic tetraphenyl borate group present in the additive (KTFPB) and hence facilities the inclusion between GEMI and HPβ-CD [16,17,21]. ...
... The resulting potential difference, formed between the phases, will then be governed by the activity of this specific ion in the two solution phases [15]. Potentiometric methods, using ion selective electrodes, have found wide application [16,17] being simple analysis procedures, economical coasts, fast results , applicable over a wide range of concentrations, applicability to various drug forms, with applicability to turbid and colored solutions, preciseness and offering enough selectivity towards the drug in the presence of various pharmaceutical excipients. Al-Mohaimeed, et al. [16] developed potentiometric sensors using different such as ion-pairing agents Phosphotungstic Acid (PTA), Phosphomolybdic Acid (PMA) and Ammonium Reineckate Salt (ARS). ...
... The membranes incorporate ion association complexes of GEMI with dibutylsebathete, dioctylphthalate, nitrophenyl octyl ether. The proposed sensors were successfully applied for determination of GEMI in bulk powder, pharmaceutical formulation, and biological fluids [17]. Research on ZnO nanostructures have been fueled by the observation that the material properties depend not only on the composition but also on the size and shape [18]. ...
... Current Trends Anal Bioanal Chem 2017, 1(1):50-56 electrode potential was observed in pH range from 2 to 3 and decreased from pH 4 to 11, Figure 4. These result suggested that the inclusion complex of GEMI and HPβCD was suitable in acidic media because GEMI containing primary amine group that capable to bind with protons presents in acidic media resulting positively charged GEMI ion, which therefore can attracted by anionic tetraphenyl borate group present in the additive (KTFPB) and hence facilities the inclusion between GEMI and HPβ-CD [16,17,21]. ...
Potentiometric method for determination of Gemifloxacin (GEMI) by ion selective electrode based on ZnO nanorods incorporation with HPβ-CD as sensing ionophore and (KTFPB) potassium tetrakis-(3,5(Triflouromethyl) Phenyl Borate) ion as anionic site (additive) in Polyvinyl Chloride (PVC) membrane, without inner reference solution was developed. The sensor shows`nearlyshows`nearly Nernstian response over a concentration range (0.5-10000 μM) with a slope of 33.65 mv decade-1 of concentration with a Limit of Detection (LOD) 0.1500 μM. The electrode exhibits a fast dynamic response of 2 s for a period of 6 months without significant change in its characteristics with excellent stability and sensitivity toward inorganic species. The method is accurate and precise as indicated by the mean recoveries 106.43% with RSD less than 2%. The proposed method was successfully applied for the determination of GEMI in pharmaceutical formulations.
... GEMI was approved by the U.S. pathogens [4]. A number of analytical methods have been reported for the determination of GEMI in pharmaceutical formulation and biological samples, including capillary electrophoresis [5,6], ion selective electrodes determination [7,8], spectrophotometric [9][10][11][12][13][14][15][16], spectrofluorometric [9,10,[15][16][17][18][19][20][21], HPLC with UV detector [22][23][24][25][26][27][28][29][30][31][32], diode-array detector [33] and HPLC with triple quadruple mass detector [34]. HPLC method with Fluorescence detector (HPLC-FL) for the determination of GEMI in spiked human plasma was demonstrated by Al-Hadiya, et al. [35]. ...
Citation: Nuha Fathi Ali Dosugi, Abdal-la A Elbashir. Development and Validation of Reverse Phase High Performance Liquid Chromatography with Fluores-cence Detector (RP-HPLC-FL) Method for the Determination of Gemifloxacin in Pharmaceutical Dosage Forms. Bi-omed J Sci & Tech Res 43(3)-2022. BJSTR. MS.ID.006895. Gemofloxacin (GEMI) is a potent antibiotic for the treatment of infection caused by gram-positive bacteria, especially streptococcus pneumonia. It is belonging to fluoroquinolone class of antibiotics and is the more active antibacterial agent among the agents in the same class. A reverse phase high performance liquid chromatography has been developed for the determination of GEMI in pharmaceutical dosage form. The separation was carried out using Hichrom packing Kromasil-100-C18 (250 mm×4.6 mm) with particle size of 5 μm and mobile phase consisting of acetonitrile: 10 mM phosphate buffer at pH 3 (15:85) at a flow rate of 1.0 mL/min. GEMI was monitored by fluorescence detector set at λex/λem 268 / 390 nm. The method was statistically validated with respect to linearity, limit of detection (LOD) and limit of quantification (LOQ), precision and accuracy. and the linearity. The method was found to be linear in concentration range of 10-150 ng/mL. The LOD and LOQ were measured to be 2.56 ng/ mL and 7.77 ng/mL, respectively. The proposed method was successfully applied for the determination of GEMI in tablets formulation.
... Many of these methods are complicated, require derivatization procedures, sophisticated instrumentation and pretreatment steps and are time and labor consuming. A literature survey showed that there were four reports for the potentiometric determination of GEMI, as shown in Table S1 [19,[26][27][28]. However, none of these electrodes were applied for the determination of GEMI in environmental samples and some of them involved the complicated and tedious procedure of manufacturing a molecularly imprinted polymer while others were liquid state ISEs which were less stable, more complicated with inner filling solution and difficult to miniaturize in comparison to their solid-contact, screen-printed counterparts developed in this work. ...
Antimicrobial resistance (AMR) is a neglected issue that poses a serious global threat to public health, causing long-term negative consequences at both humanitarian and economic levels. Herein, we report an unprecedented economic fabrication method of seven potentiometric screen-printed sensors for the ultra-trace determination of gemifloxacin (GEMI) as a model of the fluoroquinolones antibiotics deeply involved in the growing AMR problem. Sensors were constructed by depositing homemade carbon ink on a recycled X-ray sheet, patterned using stencils printed with an office printer in simple, cost-effective steps requiring no sophisticated equipment. Four sensors were modified using carbon quantum dots (CQDs) synthesized from dextrose through a single-step method. Sensors exhibited a linear response in the concentration ranges 10−5−10−2 M (sensors 1, 3 and 4), 10−6−10−3 M (sensor 2) and 10−6−10−2 M (sensors 5, 6 and 7). LOD allowed tracing of the target drug at a nano-molar level down to 210 nM. GEMI was successfully determined in pharmaceutical formulations and different water samples without any pretreatment steps with satisfactory recovery (96.93–105.28% with SD values <3). All sensors revealed a long lifetime of up to several months and are considered promising tools for monitoring water quality and efficiency of water treatment measures.
... Different analytical methods have been reported for the estimation of GFM in pharmaceutical preparations or biological fluids, namely, high-performance liquid chromatography (HPLC) [17][18][19][20][21], high-performance liquid chromatography-tandem mass spectrometry (LC-MS-MS) [22][23][24], capillary electrophoresis [25,26]), voltammetry [27][28][29], potentiometry [30,31], chemiluminescence [32], spectrophotometry [33][34][35] and spectrofluorimetry [36]. A recent study reported the synthesis of a GFM based MIP and its application as potentiometric sensor for the determination of GFM in bulk, pharmaceutical tablets and spiked human plasma [37]. ...
Eight molecularly imprinted polymers (MIPs) were synthesized for the determination of the antibacterial agent gemifloxacin mesylate (GFM). The polymers were prepared using GFM as a template, methacrylic acid (MAA) or 4-vinylpyridine (4-VP) as functional monomers, ethylene glycol dimethacrylate (EGDMA) as a cross linker, 2,2′-azobisisobutyronitrile (AIBN) as an initiator and a mixture of dimethylsulfoxide (DMSO)/acetonitrile (ACN) (1:1, v/v) as a porogen. The optimized polymer was utilized as a solid-phase extraction (SPE) sorbent material for GFM from different matrices. Different loading, washing and elution protocols were investigated. Quantitative analysis of the extracts was performed using a newly developed ultra-performance liquid chromatography–mass spectrometry (UPLC–MS/MS) method on an Acquity BEH C18 column (100 mm × 2.1 mm, particle size of 1.7 µm). The isocratic mobile phase was a mixture of methanol (MeOH)/water (H2O) with 0.1% formic acid (70:30, v/v), the flow rate was 0.3 mL min⁻¹ and the column temperature was 40 °C. Lomefloxacin (LOM) was used as an internal standard. The developed method was validated based on the recommendations of the International Conference on Harmonization (ICH) and was found suitable for the extraction of GFM from a pharmaceutical drug preparation and spiked human urine samples. Recovery % values ranged from 90.24 to 112.8% with relative standard deviation (RSD) of less than 7%.
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Five chromatographicandspectrophotometric methods have been developed for the determination of gemifloxacin (GF) in bulk powder and pharmaceutical preparations. The first method depends on RP HPLC, separation of drug& degradation products was successfully achieved on a Hypersil BDS C18 column using mobile phase consisted of citrate buffer adjusted to 2.5 PH by citric acid:Acetonitrile (70:30, v/v) at 1ml/min flow rate and 267 nm wavelength of detection. Another chromatographic method which achieved successful separation of drug& its degradation products depends on TLC densitometryusing mobile phase consisted of chloroform:methanol:toluene:diethylamine:water(33.6:33.6:16.8:10.8:6,v/v/v/v/v) with 20μl spotting volume& 260 nm wavelength of detection. Other threesimple, rapid and sensitive UV methods have been developed for GF estimation in presence ofits degradation products. One method depends on the first order derivative where GF shows sharp peak at 258.6 nm.Another method depends on derivative ratio technique by dividing the GF absorbance on that of its degradation&transforming the resulting curve into first order derivative showing a sharp peak at 285 nm. Last method depends on measuring the difference in GF absorbance in 0.1N HCL&0.1 N NaOH and transforming the difference into second order derivative showing a sharp peak at 288.2 nm. The drug follows the Beer's Lamberts for these three UV methods. The results obtained from the five proposed methods were validated statistically & by recovery studies and were found to be satisfactory.
Derivatives and their complexes from the ciprofloxacin fluoroquinoline family were synthesized, tested for antibacterial activity.The structure of derivative and their complex shows good antibacterial activity for the diagnostic aspects. Several reports have highlighted the interest of increasing the lipophilicityto improve the antitumor efficiency (2).These studies have led us to synthesize ciprofloxacin derivatives and to evaluate their activity by complex formation with metal ions. With an easy and cost-efficient procedure, derivatives of ciprofloxacin were prepared and yield had excellent.FTIR,Element Analysis, NMR analysis has been used to characterize the newly isolated complexes. This thesis intends to combine ciprofloxacin with metal ion, with the aim to improve the antibacterial activity. TheFTIR spectra of the isolated complexes suggest that ciprofloxacin derivative is act as bidentate ligands through the ring carbonyl oxygen atom and one of the oxygen atoms of the Carboxylic group. Derivative 06 showed enhanced activities than ciprofloxacin against all gram-positive and gram negative organisms likewise 2 & 5 showed highest activity against Pseudomonas spp. moreover 2 exhibited better activity against Salmonella spp, Salmonella typhi, Salmonella typhi Para-A, Salmonella typhi Para-B and Shigalla dysenteriae.
The present study describes the degradation of gemifloxacin mesylate under different International Conference on Harmonization
prescribed stress conditions (hydrolysis, oxidation, dry and wet heat and photolysis) and application of a specific and selective
stability-indicating reversed-phase liquid chromatography assay. Separation of drug and degradation products was successfully
achieved on a HiQ-SiL C8 column using 10 mM potassium dihydrogen orthophosphate (pH adjusted to 3.0 with o-phosphoric acid)–acetonitrile (65:35, v/v) at a flow rate of 1 mL min−1 and detection at 273 nm.
A simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to evaluate the accumulation of gemifloxacin in different tissues of Wister albino rat. The analytical method consists of the homogenization of tissues followed by simple liquid-liquid extraction and determination of gemifloxacin by an LC-MS/MS. The analyte was separated on a Peerless basic C(18) column (33 mm x 4.6 mm, 3 microm) with an isocratic mobile phase of methanol-water containing formic acid (1.0%, v/v) (9:1, v/v) at a flow rate of 0.6 ml/min. The MS/MS detection was carried out by monitoring the fragmentation of m/z 390.100-->372.100 for gemifloxacin and m/z 332.100-->314.200 for ciprofloxacin (internal standard; IS) on a triple quadrupole mass spectrometer. The validated method was accurate, precise and rugged with good linearity in all tissue homogenates. The accuracy and precision value obtained from six different sets of quality control samples of all tissues and serum analyzed in separate occasions within 91.833-102.283% and 0.897-5.291%, respectively. The method has been successfully applied to tissue distribution studies of gemifloxacin. The present study demonstrates that the highest tissue concentration of gemifloxacin was obtained in lung (11.891 ng/g), followed by liver (10.110 ng/g), kidney (10.095 ng/g), heart (4.251 ng/g), testis (3.750 ng/g), stomach (3.182 ng/g), adipose tissue (1.116 ng/g) and brain (0.982 ng/ml) in 3h after multiple oral dosing of 200mg gemifloxacin mesylate for 7 days. This method may also be used for gemifloxacin tissue distribution modeling study in rat tissues and antibiotic residue analyses in other animal tissues.
A new racemic fluoroquinolone antibacterial agent, gemifloxacin mesylate, has been successfully resolved on a chiral stationary phase (CSP) derived from (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid. Compared to the Crownpak CR(+) column, the CSP used in this study was more effective for the resolution of racemic gemifloxacin mesylate, especially in terms of analytical time. The resolution of gemifloxacin mesylate enantiomers on the CSP was found to be dependent on the type and content of organic and acidic modifiers in the aqueous mobile phase and the column temperature.
(+)-(18-crown-6)-tetracarboxylic acid (18C6H4) has been known as a highly efficient chiral selector for resolving primary amine enantiomers in capillary electrophoresis (CE). We investigated the chiral separation of gemifloxacin using 18C6H4 in analytical counter-current chromatography (CCC). The separation conditions for CE, including the binding constant, pH, and run buffer constituents, provided a helpful guideline for chiral CCC. A successful separation of gemifloxacin enantiomers could be achieved using a two-phase solvent system composed of 1-butanol-ethyl-acetate-bis(2-hydroxyethyl)aminotris(hydroxymethyl)methane acetate buffer with a small amount of 18C6H4. The hydrophobicity of the solvent system and the 18C6H4 concentration were varied to optimize the chiral separation.