A Selective Colorimetric Method for the Determination of Penicillins and Cephalosporins with α-Aminoacyl Functions

El-Obeid, Humeida A.; Gadkariem, Elrasheed A.; Al‐Rashood, Khalid A.; Al-Khamees, Hamad A.; El-Shafie, F. S.; Bawazeer, G.A.M.

doi:10.1080/00032719908543008

Cited by 22 publications

(14 citation statements)

References 19 publications

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“…Initially, stock solutions of the target antibiotics were prepared by dilution with methanol; however, unsatisfactory sensitivities were obtained for tetracyclines, fluoroquinolones and especially penicillins. As distilled water was employed for the preparation of penicillin standards in some previous studies (El‐Obeid et al, ; Sørensen, Rasmussen, Boison, & Keng, ), it was also utilized herein owing to the good solubility of these compounds in water. Distilled water (Halvatzis, Timotheou‐Potamia, & Calokerinos, ), methanol (Bohm et al, ) and acetonitrile (Schneider, Darwish, & Freeman, ) have been used as solvents for the preparation of stock solutions of tetracyclines; in this study, distilled water was found to be the most suitable solvent.…”

Section: Resultsmentioning

confidence: 99%

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Zheng

El‐Aty

Kim

et al. 2019

Biomedical Chromatography

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The present study was carried out to determine 16 antibiotics belonging to seven different groups (tetracyclines, sulfonamides, penicillins, fluoroquinolones, macrolides, lincosamides and trimethoprims) in duck meat. A solid‐phase extraction method based on Oasis HLB cartridges coupled with liquid chromatography–electrospray ionization tandem mass spectrometry was developed. Solutions of 0.1 m ethylenediaminetetraacetic acid disodium salt and 2% trifluoroacetic acid were used for the preliminary extraction of the target antibiotics from duck meat and n‐hexane was used for purification prior to solid‐phase extraction. Mobile phases composed of 0.1% trifluoroacetic acid in distilled water (solvent A) and 0.1% trifluoroacetic acid in methanol (solvent B), combined with a reversed‐phase C18 analytical column, provided the optimal separation and signal intensity. The linearity of the method was assessed using six concentrations (5, 10, 20, 30, 40, and 50 μg/kg), and the recoveries, which were calculated at three spiking concentrations (5, 10 and 20 μg/kg), were in the range 69.8–103.3% with relative standard deviations (RSDs) ≤ 6.9% for the 16 tested antibiotics. Matrix effects ranging from −47.2 to −13.5% were observed for all the analytes, and the limits of quantitation (LOQ), which ranged from 4.93 to 26.21 μg/kg, were much lower than the maximum residue limits (MRLs) set by various regulatory authorities. Ten samples from a market were tested, and none of the target analytes were detected. Thus, a simple and versatile protocol has been developed to detect and quantify 16 antibiotics in duck meat samples.

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Section: Resultsmentioning

confidence: 99%

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Zheng

El‐Aty

Kim

et al. 2019

Biomedical Chromatography

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“…Several analytical techniques have been applied for AMX and CLA determination in pharmaceutical and biological Abbreviations: AMX, amoxicillin; C 4 samples, such as HPLC [3][4][5][6], TLC with densitometric detection [7], UHPLC-MS/MS [8], CE with UV detection [9,10], MS [11], spectrophotometry [12,13], chemiluminescence [14], attenuated total reflectance with FTIR spectroscopy [15], sequential injection analysis [16][17][18], FIA [19], and stopped-flow techniques [20,21]. Most of the reported methods generally require expensive instrumentation and are time-consuming, which is undesirable in quality control activities.…”

Section: Introductionmentioning

confidence: 99%

Single‐run capillary electrophoresis method for the fast simultaneous determination of amoxicillin, clavulanate, and potassium

Marra

Cunha

Muñoz

et al. 2017

J of Separation Science

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We report a new fast method for the simultaneous determination of amoxicillin, clavulanate, and potassium by capillary electrophoresis with capacitively coupled contactless conductivity detection. Samples containing potassium as the cation, and both amoxicillin and clavulanate as anions were determined simultaneously in a single run (in less than 45 s) using 10 mmol/L of both 2-amino-2-hydroxymethyl-propane-1,3-diol and 3-{[2-hydroxy-1,1-bis(hydroxymethyl)ethyl]amino}-1-propanesulfonic acid (pH 8.4) as the background electrolyte. Limits of detection were 25.0, 5.0, and 4.0 μmol/L for amoxicillin, clavulanate, and potassium, respectively. The proposed method is inexpensive, simple, fast (75 injections h ), environment friendly (minimal waste generation), and accurate (recovery values between 98 and 103%). The results obtained with the proposed method were statistically similar (95% confidence level) to those obtained by using high-performance liquid chromatography (amoxicillin and clavulanate) and flame photometry (potassium).

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“…[2] Ascorbic acid was used as a colorimetric reagent after alkaline degradation. [3] 1,2-Naphthoquinone 4-sulfonate reagent was also used for the determination of cephalexin in pharmaceutical and urine samples using solid phase extraction cartridges. [4] Flow injection methods were also applied using tris(2,2-bipyridyl)ruthenium (II)-potassium permanganate systems, [5] formaldehyde-potassium permanganate system, [6] and o-phenanthroline iron system.…”

Section: Introductionmentioning

confidence: 99%

Spectrofluorometric Determination of Cephalexin in Pharmaceutical Preparations and Spiked Human Urine Using 2‐Cyanoacetamide

El‐Wasseef

2007

Spectroscopy Letters

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A simple, accurate, sensitive, and validated method was developed for the spectrofluorometric determination of cephalexin. The method involves the reaction of cephalexin with 2-cyanoacetamide in presence of 33% ammonia solution. The formed fluorescent product exhibited maximum fluorescence intensity at l 439 nm, after excitation at l 339 nm. Different experimental parameters affecting the derivatization reaction were carefully studied and incorporated in the procedure. Under the described conditions, the proposed method was linear over the concentration range 0.04-0.4 mg/ mL. The average percent found was 99.6 + 0.9%. The LOD was 7.76 ng/mL. The proposed method was applied for determination of cephalexin in pharmaceutical preparations as well as in spiked human urine. A mechanism of the reaction is postulated.

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A Selective Colorimetric Method for the Determination of Penicillins and Cephalosporins with α-Aminoacyl Functions

Cited by 22 publications

References 19 publications

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Single‐run capillary electrophoresis method for the fast simultaneous determination of amoxicillin, clavulanate, and potassium

Spectrofluorometric Determination of Cephalexin in Pharmaceutical Preparations and Spiked Human Urine Using 2‐Cyanoacetamide

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